#------------------------------------------------------------------------------
#$Date: 2018-01-01 05:21:43 +0200 (Mon, 01 Jan 2018) $
#$Revision: 204640 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/12/69/4126952.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_4126952
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, C4 H12 N'
_chemical_formula_sum            'C4 H12 Cl4 Fe N'
_chemical_formula_weight         271.80
_space_group_crystal_system      orthorhombic
_space_group_IT_number           57
_space_group_name_Hall           '-P 2c 2b'
_space_group_name_H-M_alt        'P b c m'
_symmetry_space_group_name_Hall  '-P 2c 2b'
_symmetry_space_group_name_H-M   'P b c m'
_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            4
_cell_length_a                   6.4415(15)
_cell_length_b                   13.071(3)
_cell_length_c                   14.001(3)
_cell_measurement_reflns_used    5087
_cell_measurement_temperature    250
_cell_measurement_theta_max      24.875
_cell_measurement_theta_min      2.910
_cell_volume                     1178.8(5)
_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      250
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_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  0.0422
_diffrn_reflns_av_unetI/netI     0.0210
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            15789
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.523
_diffrn_reflns_theta_min         2.910
_diffrn_source                   'rotating-anode X-ray tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.129
_exptl_absorpt_correction_T_max  0.8735
_exptl_absorpt_correction_T_min  0.6078
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/4 (Bruker,2014/4) was used for absorption correction. wR2(int) was 0.1094 before and 0.0537 after correction. The Ratio of minimum to maximum transmission is 0.6958. The λ/2 correction factor is Not present.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.531
_exptl_crystal_description       plate
_exptl_crystal_F_000             548
_exptl_crystal_size_max          0.312
_exptl_crystal_size_mid          0.087
_exptl_crystal_size_min          0.012
_refine_diff_density_max         0.480
_refine_diff_density_min         -0.362
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     53
_refine_ls_number_reflns         1411
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0625
_refine_ls_R_factor_gt           0.0445
_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)+(0.0585P)²+1.3730P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1137
_refine_ls_wR_factor_ref         0.1271
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1057
_reflns_number_total             1411
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja7b10539_si_002.cif
_cod_data_source_block           TMA_FeCl4_250K
_cod_database_code               4126952
_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   0.975
_shelx_estimated_absorpt_t_min   0.556
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2.a Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C)
;
_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+1/2, -z+1/2'
'x, -y+1/2, -z'
'-x, -y, -z'
'x, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x, 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
Fe1 Fe 0.48709(10) 0.52906(5) 0.2500 0.0492(2) Uani 1 2 d S T P
Cl1 Cl 0.5382(3) 0.69421(13) 0.2500 0.0936(6) Uani 1 2 d S T P
Cl2 Cl 0.62230(19) 0.46507(10) 0.37883(8) 0.0857(4) Uani 1 1 d . . .
Cl3 Cl 0.1543(2) 0.50044(14) 0.2500 0.0786(5) Uani 1 2 d S T P
N1 N 0.0449(7) 0.2500 0.5000 0.0562(10) Uani 1 2 d S T P
C1 C -0.0862(11) 0.2011(6) 0.4281(4) 0.128(2) Uani 1 1 d . . .
H1A H -0.1865 0.1571 0.4595 0.191 Uiso 1 1 calc GR . .
H1B H -0.0005 0.1606 0.3856 0.191 Uiso 1 1 calc GR . .
H1C H -0.1586 0.2532 0.3917 0.191 Uiso 1 1 calc GR . .
C2 C 0.1688(13) 0.3278(6) 0.4555(5) 0.159(3) Uani 1 1 d . . .
H2A H 0.2262 0.3724 0.5042 0.238 Uiso 1 1 calc GR . .
H2B H 0.0830 0.3676 0.4124 0.238 Uiso 1 1 calc GR . .
H2C H 0.2808 0.2961 0.4200 0.238 Uiso 1 1 calc GR . .
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
Cl2 Fe1 Cl1 108.69(5) . .
Cl2 Fe1 Cl1 108.69(5) 6_556 .
Cl2 Fe1 Cl2 112.39(8) . 6_556
Cl2 Fe1 Cl3 109.21(5) . .
Cl2 Fe1 Cl3 109.21(5) 6_556 .
Cl3 Fe1 Cl1 108.57(8) . .
C1 N1 C1 109.4(6) . 4_556
C2 N1 C1 108.1(5) 4_556 .
C2 N1 C1 109.4(4) 4_556 4_556
C2 N1 C1 108.1(5) . 4_556
C2 N1 C1 109.4(4) . .
C2 N1 C2 112.4(8) 4_556 .
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 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 Cl1 2.1836(18) .
Fe1 Cl2 2.1706(12) 6_556
Fe1 Cl2 2.1706(12) .
Fe1 Cl3 2.1764(16) .
N1 C1 1.461(6) 4_556
N1 C1 1.461(6) .
N1 C2 1.435(6) .
N1 C2 1.435(6) 4_556
C1 H1A 0.9700 .
C1 H1B 0.9700 .
C1 H1C 0.9700 .
C2 H2A 0.9700 .
C2 H2B 0.9700 .
C2 H2C 0.9700 .
