#------------------------------------------------------------------------------
#$Date: 2018-01-01 05:23:04 +0200 (Mon, 01 Jan 2018) $
#$Revision: 204642 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/12/69/4126954.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_4126954
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), 0.25(C12 H36 N4), C'
_chemical_formula_sum            'C4 H12 Cl4 Fe N'
_chemical_formula_weight         271.80
_space_group_crystal_system      orthorhombic
_space_group_IT_number           63
_space_group_name_Hall           '-C 2c 2'
_space_group_name_H-M_alt        'C m c m'
_symmetry_space_group_name_Hall  '-C 2c 2'
_symmetry_space_group_name_H-M   'C m c m'
_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            4
_cell_length_a                   8.964(9)
_cell_length_b                   9.618(9)
_cell_length_c                   14.158(13)
_cell_measurement_reflns_used    3586
_cell_measurement_temperature    360
_cell_measurement_theta_max      24.581
_cell_measurement_theta_min      2.877
_cell_volume                     1221(2)
_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      360
_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  0.0350
_diffrn_reflns_av_unetI/netI     0.0146
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            9245
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.532
_diffrn_reflns_theta_min         2.877
_diffrn_source                   'rotating-anode X-ray tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.056
_exptl_absorpt_correction_T_max  0.704093
_exptl_absorpt_correction_T_min  0.549358
_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 0.1013 before and 0.0450 after correction.
 The Ratio of minimum to maximum transmission is 0.78.
 The λ/2 correction factor is Not present
 
For component 2:
 wR2(int) was 0.1076 before and 0.0449 after correction.
 The Ratio of minimum to maximum transmission is 0.78.
 The λ/2 correction factor is Not present

Final HKLF 4 output contains 9245 reflections, Rint = 0.0350
 (5220 with I > 3sig(I), Rint = 0.0318)
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.479
_exptl_crystal_description       block
_exptl_crystal_F_000             548
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.188
_exptl_crystal_size_min          0.125
_refine_diff_density_max         0.483
_refine_diff_density_min         -0.224
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     57
_refine_ls_number_reflns         785
_refine_ls_number_restraints     45
_refine_ls_restrained_S_all      1.148
_refine_ls_R_factor_all          0.0795
_refine_ls_R_factor_gt           0.0636
_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)+(0.1031P)²+1.4299P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1943
_refine_ls_wR_factor_ref         0.2068
_reflns_Friedel_coverage         0.000
_reflns_number_gt                577
_reflns_number_total             785
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja7b10539_si_005.cif
_cod_data_source_block           TMA_FeCl4_360K
_cod_database_code               4126954
_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. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N1-C1 \\sim N1-C2 \\sim N1-C3 \\sim N1-C4
 with sigma of 0.02
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(0.25) H1A(0.25) H1B(0.25) H1C(0.25) C2(0.25) H2A(0.25)
 H2B(0.25) H2C(0.25) C3(0.25) H3A(0.25) H3B(0.25) H3C(0.25) C4(0.25) H4A(0.25)
 H4B(0.25) H4C(0.25)
5.a Me refined with riding coordinates:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C3(H3A,H3B,H3C)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'-x, y, -z+1/2'
'x, -y, -z'
'x+1/2, y+1/2, 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'
'-x, -y, -z'
'x, y, -z-1/2'
'x, -y, z-1/2'
'-x, y, z'
'-x+1/2, -y+1/2, -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'
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 0.0000 0.56927(12) 0.2500 0.0854(6) Uani 1 4 d S TU P . .
Cl1 Cl 0.1971(4) 0.7008(3) 0.2500 0.1739(13) Uani 1 2 d S TU P . .
Cl2 Cl 0.0000 0.4449(3) 0.37652(17) 0.1504(11) Uani 1 2 d S TU P . .
N1 N 0.5000 0.5000 0.5000 0.100(2) Uani 1 4 d DS TU P . .
C1 C 0.412(4) 0.373(3) 0.522(3) 0.156(8) Uani 0.25 1 d D U P A -1
H1A H 0.3110 0.3982 0.5370 0.234 Uiso 0.25 1 calc R U P A -1
H1B H 0.4113 0.3124 0.4675 0.234 Uiso 0.25 1 calc R U P A -1
H1C H 0.4557 0.3249 0.5743 0.234 Uiso 0.25 1 calc R U P A -1
C2 C 0.652(2) 0.446(3) 0.478(3) 0.155(8) Uani 0.25 1 d D U P A -1
H2A H 0.6431 0.3635 0.4402 0.233 Uiso 0.25 1 calc R U P A -1
H2B H 0.7061 0.5154 0.4430 0.233 Uiso 0.25 1 calc R U P A -1
H2C H 0.7033 0.4254 0.5353 0.233 Uiso 0.25 1 calc R U P A -1
C3 C 0.439(4) 0.621(3) 0.554(3) 0.159(9) Uani 0.25 1 d D U P A -1
H3A H 0.3318 0.6184 0.5513 0.239 Uiso 0.25 1 calc R U P A -1
H3B H 0.4712 0.6155 0.6181 0.239 Uiso 0.25 1 calc R U P A -1
H3C H 0.4740 0.7056 0.5258 0.239 Uiso 0.25 1 calc R U P A -1
C4 C 0.437(3) 0.528(3) 0.4026(14) 0.141(7) Uani 0.25 1 d D U P A -1
H4A H 0.3375 0.5643 0.4084 0.211 Uiso 0.25 1 calc R U P A -1
H4B H 0.4986 0.5955 0.3709 0.211 Uiso 0.25 1 calc R U P A -1
H4C H 0.4352 0.4437 0.3668 0.211 Uiso 0.25 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
_geom_angle_site_symmetry_3
Cl1 Fe1 Cl1 108.8(2) . 3
Cl2 Fe1 Cl1 108.86(7) 10_556 3
Cl2 Fe1 Cl1 108.86(7) 10_556 .
Cl2 Fe1 Cl1 108.86(7) . .
Cl2 Fe1 Cl1 108.86(7) . 3
Cl2 Fe1 Cl2 112.53(19) 10_556 .
C1 N1 C4 98(2) . .
C2 N1 C1 104(2) . .
C2 N1 C3 135.6(16) . .
C2 N1 C4 102(2) . .
C3 N1 C1 109.9(17) . .
C3 N1 C4 100.7(19) . .
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 . .
H2A C2 H2B 109.5 . .
H2A C2 H2C 109.5 . .
H2B C2 H2C 109.5 . .
N1 C3 H3A 109.5 . .
N1 C3 H3B 109.5 . .
N1 C3 H3C 109.5 . .
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 2.173(3) 3
Fe1 Cl1 2.173(3) .
Fe1 Cl2 2.154(3) .
Fe1 Cl2 2.154(3) 10_556
N1 C1 1.492(16) .
N1 C2 1.487(16) .
N1 C3 1.491(16) .
N1 C4 1.515(16) .
C1 H1A 0.9600 .
C1 H1B 0.9600 .
C1 H1C 0.9600 .
C2 H2A 0.9600 .
C2 H2B 0.9600 .
C2 H2C 0.9600 .
C3 H3A 0.9600 .
C3 H3B 0.9600 .
C3 H3C 0.9600 .
C4 H4A 0.9600 .
C4 H4B 0.9600 .
C4 H4C 0.9600 .
