#------------------------------------------------------------------------------
#$Date: 2019-12-26 21:19:10 +0200 (Thu, 26 Dec 2019) $
#$Revision: 246094 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/31/17/2311722.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2311722
loop_
_publ_author_name
'Binns, Jack'
'McIntyre, Garry J.'
'Barreda-Argüeso, José A'
'González, Jesús'
'Aguado, Fernando'
'Rodríguez, Fernando'
'Valiente, Rafael'
'Parsons, Simon'
_publ_section_title
;
 Phase transition sequences in tetramethylammonium tetrachlorometallates
 by X-ray diffraction and spectroscopic measurements.
;
_journal_issue                   'Pt 5'
_journal_name_full
'Acta crystallographica Section B, Structural science, crystal engineering and materials'
_journal_page_first              844
_journal_page_last               855
_journal_paper_doi               10.1107/S2052520617006412
_journal_volume                  73
_journal_year                    2017
_chemical_formula_moiety         'C4 H12 N1, Cl4 Fe1'
_chemical_formula_sum            'C4 H12 Cl4 Fe N'
_chemical_formula_weight         271.8045
_chemical_name_systematic        'tetramethylammonium tetrachloroferrate(III)'
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             15-09-23
_audit_creation_method           CRYSTALS_ver_14.40
_cell_angle_alpha                90
_cell_angle_beta                 93.87(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   6.574(3)
_cell_length_b                   14.156(7)
_cell_length_c                   6.595(3)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    365
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_volume                     612.3(5)
_computing_cell_refinement       'CrysAlis, (Oxford Diffraction, 2002)'
_computing_data_collection       'SuperNova, (Oxford Diffraction, 2010)'
_computing_data_reduction        'CrysAlis, (Oxford Diffraction, 2002)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      365
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Oxford Diffraction SuperNova'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.065
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            5173
_diffrn_reflns_theta_full        19.861
_diffrn_reflns_theta_max         20.907
_diffrn_reflns_theta_min         3.106
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.047
_exptl_absorpt_correction_T_max  0.90
_exptl_absorpt_correction_T_min  0.49
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis, (Oxford Diffraction, 2002)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.474
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             250
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.59
_refine_diff_density_min         -0.62
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0450
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     32
_refine_ls_number_reflns         665
_refine_ls_number_restraints     17
_refine_ls_R_factor_all          0.1330
_refine_ls_R_factor_gt           0.1190
_refine_ls_shift/su_max          0.0000089
_refine_ls_shift/su_mean         0.0000021
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A₀*T₀(x)+A₁*T₁(x) ... +Aₙ₋₁]*Tₙ₋₁(x)] 
 where Ai are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)²]² 
 Ai are: 
 48.0 59.4 18.0 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2057
_refine_ls_wR_factor_gt          0.2006
_refine_ls_wR_factor_ref         0.2055
_reflns_limit_h_max              6
_reflns_limit_h_min              -6
_reflns_limit_k_max              14
_reflns_limit_k_min              0
_reflns_limit_l_max              6
_reflns_limit_l_min              0
_reflns_number_gt                576
_reflns_number_total             675
_reflns_threshold_expression     I>2.0σ(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_r_factor_ref   0.1328
_oxford_refine_ls_scale          1.06(2)
_oxford_reflns_number_all        666
_oxford_reflns_threshold_expression_ref I>0.0\s(I)
_oxford_structure_analysis_title 'JB15_P21m in P2(1)/m'
_cod_data_source_file            fx5008sup1.cif
_cod_data_source_block           TCF_mP44_365
_cod_original_sg_symbol_H-M      'P 1 21/m 1 '
_cod_original_formula_sum        'C4 H12 Cl4 Fe1 N1'
_cod_database_code               2311722
_iucr_refine_instructions_details_constraints
;
#
# Punched on 23/09/15 at 11:27:05
#
#LIST     12                                                                    
BLOCK 
CONT SCALE 
CONT FE   (    1 ,X'S,U'S)  UNTIL CL   (    3 ) 
CONT N    (    1 ,X'S,U[ISO]) 
CONT C    (    100 ,U[ISO],SIZE) 
SUMFIX ELEMENT SCALES 
END                                                                             
;
_iucr_refine_instructions_details_restraints
;
#
# Punched on 23/09/15 at 11:27:05
#
#LIST     16                                                                    
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
DISTANCE 1.450000 , 0.050000 = N(1) TO C(10) 
DISTANCE 1.450000 , 0.050000 = N(1) TO C(3) 
REM   DELU   START (DO NOT REMOVE THIS LINE) 
VIBR .0, 0.00200 = FE(1) TO CL(2,-2,1,0,1) 
VIBR .0, 0.00200 = FE(1) TO CL(2) 
VIBR .0, 0.00200 = FE(1) TO CL(3) 
VIBR .0, 0.00200 = FE(1) TO CL(4) 
VIBR .0, 0.00500 = CL(2) TO CL(2,-2,1,0,1) 
VIBR .0, 0.00500 = CL(3) TO CL(2,-2,1,0,1) 
VIBR .0, 0.00500 = CL(3) TO CL(2) 
VIBR .0, 0.00500 = CL(4) TO CL(2,-2,1,0,1) 
VIBR .0, 0.00500 = CL(4) TO CL(2) 
VIBR .0, 0.00500 = CL(4) TO CL(3) 
REM   DELU   END (DO NOT REMOVE THIS LINE) 
REM   THERMSIM   START (DO NOT REMOVE THIS LINE) 
U(IJ) .0, 0.04000 = FE(1) TO CL(2,-2,1,0,1) 
U(IJ) .0, 0.04000 = FE(1) TO CL(2) 
U(IJ) .0, 0.08000 = FE(1) TO CL(3) 
U(IJ) .0, 0.08000 = FE(1) TO CL(4) 
REM   THERMSIM   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
-x,y+1/2,-z
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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
Fe1 Fe -0.0676(10) 0.2500 0.0686(9) 0.0980 1.0000 Uani S TU
Cl1 Cl 0.0464(18) 0.1232(5) -0.0569(15) 0.1608 1.0000 Uani . .
Cl2 Cl -0.032(3) 0.2500 0.3879(19) 0.1317 1.0000 Uani S TU
Cl3 Cl -0.405(3) 0.2500 -0.023(3) 0.1727 1.0000 Uani S TU
N1 N 0.5000 0.0000 0.5000 0.103(7) 1.0000 Uiso DS .
C100 C 0.5000 0.0000 0.5000 0.103(19) 4.0000 Uiso . .
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 0.101(7) 0.109(3) 0.084(5) 0.0000 0.003(2) 0.0000
Cl1 0.226(19) 0.096(4) 0.158(14) -0.003(6) -0.005(5) 0.067(7)
Cl2 0.195(12) 0.115(3) 0.084(5) 0.0000 0.004(6) 0.0000
Cl3 0.119(9) 0.139(5) 0.251(18) 0.0000 -0.056(10) 0.0000
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Cl 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784
-9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Fe 0.3463 0.8444 11.7695 4.7611 7.3573 0.3072 3.5222 15.3535 2.3045 76.8805
1.0369 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_publ_flag
Cl1 4_555 Fe1 Cl1 114.5(5) yes
Cl1 4_555 Fe1 Cl2 111.7(4) yes
Cl1 . Fe1 Cl2 111.7(4) yes
Cl1 4_555 Fe1 Cl3 105.1(5) yes
Cl1 . Fe1 Cl3 105.1(5) yes
Cl2 . Fe1 Cl3 108.0(5) yes
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Fe1 Cl1 4_555 2.133(6) yes
Fe1 Cl1 . 2.133(6) yes
Fe1 Cl2 . 2.103(13) yes
Fe1 Cl3 . 2.259(17) yes
loop_
_oxford_atom_site_label
_oxford_atom_site_special_uiso
_oxford_atom_site_special_size
_oxford_atom_site_special_shape
C100 0.103(19) 1.55(2) Sphere
loop_
_oxford_twin_element_scale_factors
0.508(18)
0.496(18)
loop_
_oxford_refln_omitted_index_h
_oxford_refln_omitted_index_k
_oxford_refln_omitted_index_l
_oxford_refln_omitted_flag
-1 0 1 x
0 2 1 x
1 2 0 x
1 0 1 x
1 5 1 x
-1 8 1 x
