# Electronic Supplementary Material (ESI) for RSC Advances.
# This journal is © The Royal Society of Chemistry 2020

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Compound1_400K
_database_code_depnum_ccdc_archive 'CCDC 1897672'
loop_
_audit_author_name
_audit_author_address
'Garikoitz Beobide'
;Universidad del Pais Vasco
Spain
;
_audit_update_record             
;
2019-02-17 deposited with the CCDC.	2020-03-09 downloaded from the CCDC.
;

_audit_creation_method           
'Created with CONVERT.DLL (www.crystalimpact.com)'
_audit_creation_date             2018-08-29

_chemical_name_systematic        
;
1,2,3-trimethylimidazolium tetrachlorideferrate(III) 
;
_chemical_formula_moiety         'C6 H11 N2, Cl4 Fe'
_chemical_formula_sum            'C6 H11 Cl4 Fe N2'
_chemical_formula_weight         308.82

#==============================================================================
# POWDER SPECIMEN AND CRYSTAL DATA

_space_group_crystal_system      orthorhombic
_symmetry_int_tables_number      60
_symmetry_space_group_name_H-M   'P b c n'
_symmetry_space_group_name_Hall  -P_2n_2ab

loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 1/2-x,1/2-y,1/2+z
3 1/2+x,1/2-y,-z
4 -x,y,1/2-z
5 -x,-y,-z
6 1/2+x,1/2+y,1/2-z
7 1/2-x,1/2+y,z
8 x,-y,1/2+z

_cell_length_a                   10.4559(1)
_cell_length_b                   9.2217(1)
_cell_length_c                   14.0803(2)
_cell_angle_alpha                90.000
_cell_angle_beta                 90.000
_cell_angle_gamma                90.000
_cell_volume                     1357.63(3)

_cell_formula_units_Z            4
_cell_measurement_temperature    400
_exptl_crystal_density_diffrn    1.511

_exptl_crystal_F_000             620
_exptl_absorpt_coefficient_mu    1.248
_exptl_absorpt_correction_type   none

_pd_spec_mounting                'glass capillary'
_pd_spec_mount_mode              transmission

#==============================================================================
# EXPERIMENTAL DATA

_diffrn_ambient_temperature      400
_diffrn_measurement_device_type  'BL04 - MSPD'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.61872

_diffrn_radiation_monochromator  'Si (111)'
_diffrn_detector                 MYTHEN-II
_pd_instr_location               
;
'BL04-MSPD, ALBA Synchrotron Light Source (SPAIN)'
;

#  Measured (not processed) powder pattern details.  Angles are in degrees.
_pd_meas_number_of_points        7138
_pd_meas_2theta_range_min        0.726
_pd_meas_2theta_range_max        43.548
_pd_meas_2theta_range_inc        0.006

_computing_data_reduction        'DAJUST (Vallcorba et al., 2012)'
_computing_structure_solution    'TALP (Vallcorba et al., 2012)'
_computing_structure_refinement  'RIBOLS (Rius, 2012)'
_computing_publication_material  'PLATON (Spek, 2003)'

#==============================================================================
# REFINEMENT

_pd_proc_ls_profile_function     Pseudo-Voigt
_pd_proc_ls_background_function  'Smoothing procedure (Br\"uckner, 2004)'
_pd_proc_ls_prof_wR_factor       0.065
_refine_ls_R_I_factor            0.078
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     1/Yobs
_refine_ls_hydrogen_treatment    noref
_refine_ls_number_reflns         431
_refine_ls_number_parameters     43
_refine_ls_number_restraints     30
_refine_ls_goodness_of_fit_all   3.999
_refine_ls_shift/su_max          0.043
_refine_ls_shift/su_mean         0.019

_pd_proc_number_of_points        4651
_pd_proc_2theta_range_min        2.500
_pd_proc_2theta_range_max        30.400
_pd_proc_2theta_range_inc        0.006

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_Wyckoff_symbol
_atom_site_calc_flag
_atom_site_U_iso_or_equiv
_atom_site_disorder_group
Fe01 Fe 1.00000 0.7948(4) 0.25000 1.0000 4 c d 0.115(4) .
Cl1 Cl 1.0040(9) 0.9307(4) 0.1258(4) 1.0000 8 d d 0.155(3) .
Cl2 Cl 0.8272(3) 0.6606(4) 0.2530(4) 1.0000 8 d d 0.155(3) .
N11 N 0.4538(31) -0.0826(23) 0.4528(4) 0.5000 8 d d 0.211(4) -1
C12 C 0.5596(32) -0.0271(20) 0.4909(4) 0.5000 8 d d 0.211(4) -1
N13 N 0.5297(34) 0.0796(21) 0.5483(4) 0.5000 8 d d 0.211(4) -1
C14 C 0.3969(34) 0.0889(25) 0.5445(4) 0.5000 8 d d 0.211(4) -1
H14 H 0.3487 0.1560 0.5784 0.5000 8 d c 0.211 -1
C15 C 0.3458(32) -0.0092(27) 0.4864(4) 0.5000 8 d d 0.211(4) -1
H15 H 0.2604 -0.0254 0.4715 0.5000 8 d c 0.211(4) -1
C16 C 0.4485(33) -0.2010(23) 0.3860(4) 0.5000 8 d d 0.211(4) -1
H16a H 0.3611 -0.2204 0.3694 0.5000 8 d c 0.211 -1
H16b H 0.4956 -0.1761 0.3298 0.5000 8 d c 0.211 -1
H16c H 0.4855 -0.2857 0.4145 0.5000 8 d c 0.211 -1
C17 C 0.6886(32) -0.0817(19) 0.4691(4) 0.5000 8 d d 0.211(4) -1
H17a H 0.7525 -0.0279 0.5031 0.5000 8 d c 0.211 -1
H17b H 0.6931 -0.1820 0.4870 0.5000 8 d c 0.211 -1
H17c H 0.7035 -0.0727 0.4021 0.5000 8 d c 0.211 -1
C18 C 0.6100(37) 0.1707(20) 0.6050(4) 0.5000 8 d d 0.211(4) -1
H18a H 0.5556 0.2376 0.6381 0.5000 8 d c 0.211 -1
H18b H 0.6574 0.1142 0.6502 0.5000 8 d c 0.211 -1
H18c H 0.6683 0.2235 0.5653 0.5000 8 d c 0.211 -1

#===============================================================================
# MOLECULAR GEOMETRY

_geom_special_details            
;
 Bond distances, angles etc. have been calculated using the
 rounded fractional coordinates. All su's are estimated
 from the variances of the (full) variance-covariance matrix.
 The cell esds are taken into account in the estimation of
 distances, angles and torsion angles
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe01 Cl1 2.152(5) . . ?
Fe01 Cl2 2.190(4) . . ?
N11 C12 1.34(4) . . ?
N11 C15 1.40(4) . . ?
N11 C16 1.44(2) . . ?
N13 C12 1.31(2) . . ?
N13 C14 1.39(4) . . ?
N13 C18 1.43(3) . . ?
C12 C17 1.47(4) . . ?
C14 C15 1.33(3) . . ?
C14 H14 0.9300 . . ?
C15 H15 0.9300 . . ?
C16 H16A 0.9700 . . ?
C16 H16B 0.9600 . . ?
C16 H16C 0.9600 . . ?
C17 H17A 0.9600 . . ?
C17 H17B 0.9600 . . ?
C17 H17C 0.9600 . . ?
C18 H18A 0.9600 . . ?
C18 H18B 0.9600 . . ?
C18 H18C 0.9600 . . ?

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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cl1 Fe01 Cl2 111.2(3) . . . ?
C12 N11 C15 110.2(17) . . . ?
C12 N11 C16 126(3) . . . ?
C15 N11 C16 124(3) . . . ?
C12 N13 C14 105(2) . . . ?
C12 N13 C18 130(3) . . . ?
C14 N13 C18 125(2) . . . ?
N11 C12 N13 110(3) . . . ?
N11 C12 C17 123.0(16) . . . ?
N13 C12 C17 127(2) . . . ?
N13 C14 C15 113(2) . . . ?
N11 C15 C14 102(3) . . . ?
N13 C14 H14 124.00 . . . ?
C15 C14 H14 123.00 . . . ?
N11 C15 H15 128.00 . . . ?
C14 C15 H15 129.00 . . . ?
N11 C16 H16A 109.00 . . . ?
N11 C16 H16B 110.00 . . . ?
N11 C16 H16C 109.00 . . . ?
H16A C16 H16B 109.00 . . . ?
H16A C16 H16C 109.00 . . . ?
H16B C16 H16C 110.00 . . . ?
C12 C17 H17A 111.00 . . . ?
C12 C17 H17B 108.00 . . . ?
C12 C17 H17C 109.00 . . . ?
H17A C17 H17B 110.00 . . . ?
H17A C17 H17C 110.00 . . . ?
H17B C17 H17C 110.00 . . . ?
N13 C18 H18A 108.00 . . . ?
N13 C18 H18B 111.00 . . . ?
N13 C18 H18C 110.00 . . . ?
H18A C18 H18B 109.00 . . . ?
H18A C18 H18C 110.00 . . . ?
H18B C18 H18C 109.00 . . . ?
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Compound1_150K
_database_code_depnum_ccdc_archive 'CCDC 1897674'
loop_
_audit_author_name
_audit_author_address
'Garikoitz Beobide'
;Universidad del Pais Vasco
Spain
;
_audit_update_record             
;
2019-02-17 deposited with the CCDC.	2020-03-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7

_chemical_name_systematic        
;
1,2,3-trimethylimidazolium tetrachlorideferrate(III) 
;
_chemical_formula_moiety         'C6 H11 N2, Cl4 Fe'
_chemical_formula_sum            'C6 H11 Cl4 Fe N2'
_chemical_formula_weight         308.82

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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   6.541(5)
_cell_length_b                   14.158(5)
_cell_length_c                   13.351(5)
_cell_angle_alpha                90.000
_cell_angle_beta                 95.590(5)
_cell_angle_gamma                90.000
_cell_volume                     1230.5(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    2627
_cell_measurement_theta_min      0.72416
_cell_measurement_theta_max      1.00000

_exptl_crystal_description       prismatic
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.667
_exptl_crystal_F_000             620
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.11
_exptl_absorpt_coefficient_mu    2.053
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_absorpt_correction_T_min  0.72416
_exptl_absorpt_correction_T_max  1.0000


_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'SuperNova (Mo) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       ω
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            8114
_diffrn_reflns_av_unetI/netI     0.0412
_diffrn_reflns_av_R_equivalents  0.0484
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.102
_diffrn_reflns_theta_max         26.619
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             2542
_reflns_number_gt                2028
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
;
_computing_structure_solution    'Sir92 (Altomare et al., 1993)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_molecular_graphics    'Ortep-3 (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_refine_special_details          
;
 Refinement of F² against ALL reflections. The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement. R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
PLATON  Addsym routine detects a possible pseudo-translation (c/2) at 0 -0.004 1/2, but the nonfits (ca. 8%) include C5 atom of the imidazolic ring, which implies to rule out the proposition. In fact, its consideration leads to persistently high R1 values (12-13%) and the resulting structure require modelling a disorder of imidazolium cation in two positions. Furthermore, the thermal parameters of the disordered atoms are not clearly defined and require hard restrains to make the refinement stable. All in all, proposed pseudo-translation has been disregarded, in such a way that the herein reported structure is featured by lacking of any disordered entity and by exhbiting reasonable R-factors (R1 = 5.3%) and anisotropic thermal displacement parameters.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0528P)²+3.3176P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2542
_refine_ls_number_parameters     121
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0658
_refine_ls_R_factor_gt           0.0528
_refine_ls_wR_factor_ref         0.1445
_refine_ls_wR_factor_gt          0.1365
_refine_ls_goodness_of_fit_ref   1.158
_refine_ls_restrained_S_all      1.158
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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 0.74428(9) 0.75192(4) 0.88895(5) 0.0201(2) Uani 1 1 d . . . . .
Cl14 Cl 0.42734(15) 0.74819(7) 0.93132(9) 0.0260(3) Uani 1 1 d . . . . .
Cl13 Cl 0.74253(18) 0.75467(8) 0.72461(8) 0.0266(3) Uani 1 1 d . . . . .
Cl12 Cl 0.89277(15) 0.88225(7) 0.94844(8) 0.0237(3) Uani 1 1 d . . . . .
Cl11 Cl 0.90464(17) 0.62405(8) 0.94567(9) 0.0275(3) Uani 1 1 d . . . . .
N3 N 0.6238(5) 0.4616(3) 0.7444(3) 0.0233(8) Uani 1 1 d . . . . .
N1 N 0.3856(6) 0.5614(2) 0.6976(3) 0.0189(7) Uani 1 1 d . . . . .
C7 C 0.3647(8) 0.4906(3) 0.8676(3) 0.0299(10) Uani 1 1 d . . . . .
H7A H 0.4355 0.4408 0.9054 0.045 Uiso 1 1 calc R U . . .
H7B H 0.2222 0.4744 0.8541 0.045 Uiso 1 1 calc R U . . .
H7C H 0.3772 0.5482 0.9058 0.045 Uiso 1 1 calc R U . . .
C6 C 0.2026(7) 0.6209(3) 0.6965(4) 0.0311(11) Uani 1 1 d . . . . .
H6A H 0.0830 0.5817 0.6971 0.047 Uiso 1 1 calc R U . . .
H6B H 0.1907 0.6592 0.6369 0.047 Uiso 1 1 calc R U . . .
H6C H 0.2139 0.6609 0.7549 0.047 Uiso 1 1 calc R U . . .
C5 C 0.5119(8) 0.5554(3) 0.6216(3) 0.0292(10) Uani 1 1 d . . . . .
H5 H 0.4972 0.5884 0.5611 0.035 Uiso 1 1 calc R U . . .
C2 C 0.4552(6) 0.5037(3) 0.7723(3) 0.0166(8) Uani 1 1 d . . . . .
C4 C 0.6590(8) 0.4938(3) 0.6504(4) 0.0305(11) Uani 1 1 d . . . . .
H4 H 0.7664 0.4758 0.6137 0.037 Uiso 1 1 calc R U . . .
C8 C 0.7521(8) 0.3942(4) 0.8050(5) 0.0430(14) Uani 1 1 d . . . . .
H8A H 0.8253 0.4266 0.8606 0.064 Uiso 1 1 calc R U . . .
H8B H 0.8484 0.3658 0.7642 0.064 Uiso 1 1 calc R U . . .
H8C H 0.6669 0.3461 0.8299 0.064 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 Cl11 2.1901(13) . ?
Fe1 Cl13 2.1934(15) . ?
Fe1 Cl12 2.1974(13) . ?
Fe1 Cl14 2.2021(19) . ?
N3 C2 1.338(5) . ?
N3 C4 1.376(6) . ?
N3 C8 1.461(6) . ?
N1 C2 1.335(5) . ?
N1 C5 1.371(6) . ?
N1 C6 1.462(6) . ?
C7 C2 1.467(6) . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C5 C4 1.327(7) . ?
C5 H5 0.9300 . ?
C4 H4 0.9300 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?

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
_geom_angle_publ_flag
Cl11 Fe1 Cl13 108.43(5) . . ?
Cl11 Fe1 Cl12 112.91(6) . . ?
Cl13 Fe1 Cl12 107.80(5) . . ?
Cl11 Fe1 Cl14 108.81(6) . . ?
Cl13 Fe1 Cl14 110.13(5) . . ?
Cl12 Fe1 Cl14 108.74(5) . . ?
C2 N3 C4 108.8(4) . . ?
C2 N3 C8 125.5(4) . . ?
C4 N3 C8 125.7(4) . . ?
C2 N1 C5 109.2(4) . . ?
C2 N1 C6 125.4(4) . . ?
C5 N1 C6 125.5(4) . . ?
C2 C7 H7A 109.5 . . ?
C2 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C2 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N1 C6 H6A 109.5 . . ?
N1 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
N1 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C4 C5 N1 107.4(4) . . ?
C4 C5 H5 126.3 . . ?
N1 C5 H5 126.3 . . ?
N1 C2 N3 107.2(4) . . ?
N1 C2 C7 126.1(4) . . ?
N3 C2 C7 126.8(4) . . ?
C5 C4 N3 107.5(4) . . ?
C5 C4 H4 126.3 . . ?
N3 C4 H4 126.3 . . ?
N3 C8 H8A 109.5 . . ?
N3 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
N3 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?

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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C2 N1 C5 C4 -0.1(5) . . . . ?
C6 N1 C5 C4 -179.5(4) . . . . ?
C5 N1 C2 N3 0.1(4) . . . . ?
C6 N1 C2 N3 179.6(4) . . . . ?
C5 N1 C2 C7 179.1(4) . . . . ?
C6 N1 C2 C7 -1.4(7) . . . . ?
C4 N3 C2 N1 -0.1(5) . . . . ?
C8 N3 C2 N1 178.5(4) . . . . ?
C4 N3 C2 C7 -179.1(4) . . . . ?
C8 N3 C2 C7 -0.5(7) . . . . ?
N1 C5 C4 N3 0.0(5) . . . . ?
C2 N3 C4 C5 0.0(5) . . . . ?
C8 N3 C4 C5 -178.5(4) . . . . ?

_refine_diff_density_max         0.925
_refine_diff_density_min         -0.824
_refine_diff_density_rms         0.133

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_compound1_250K
_database_code_depnum_ccdc_archive 'CCDC 1897673'
loop_
_audit_author_name
_audit_author_address
'Garikoitz Beobide'
;Universidad del Pais Vasco
Spain
;
_audit_update_record             
;
2019-02-17 deposited with the CCDC.	2020-03-09 downloaded from the CCDC.
;

_chemical_name_systematic        
;
1,2,3-trimethylimidazolium tetrachlorideferrate(III) 
;
_chemical_formula_moiety         'C6 H11 N2, Cl4 Fe'
_chemical_formula_sum            'C6 H11 Cl4 Fe N2'
_chemical_formula_weight         308.82

#==============================================================================
# POWDER SPECIMEN AND CRYSTAL DATA

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_int_tables_number      14

loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 -x,y+1/2,-z+1/2
3 -x,-y,-z
4 x,-y+1/2,z+1/2

_cell_length_a                   6.6159(2)
_cell_length_b                   14.2024(3)
_cell_length_c                   13.5728(3)
_cell_angle_alpha                90.0000
_cell_angle_beta                 95.905(2)
_cell_angle_gamma                90.0000
_cell_volume                     1268.56(5)

_cell_formula_units_Z            4
_cell_measurement_temperature    250
_exptl_crystal_density_diffrn    1.617

_exptl_crystal_F_000             620
_exptl_absorpt_coefficient_mu    1.335
_exptl_absorpt_correction_type   none

_pd_spec_mounting                'glass capillary'
_pd_spec_mount_mode              transmission

#==============================================================================
# EXPERIMENTAL DATA

_diffrn_ambient_temperature      250
_diffrn_measurement_device_type  'BL04 - MSPD'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.61872

_diffrn_radiation_monochromator  'Si (111)'
_diffrn_detector                 MYTHEN-II
_pd_instr_location               
;
'BL04-MSPD, ALBA Synchrotron Light Source (SPAIN)'
;

#  Measured (not processed) powder pattern details.  Angles are in degrees.
_pd_meas_number_of_points        7138
_pd_meas_2theta_range_min        0.726
_pd_meas_2theta_range_max        43.548
_pd_meas_2theta_range_inc        0.006

_computing_data_reduction        'DAJUST (Vallcorba et al., 2012)'
_computing_structure_solution    'TALP (Vallcorba et al., 2012)'
_computing_structure_refinement  'RIBOLS (Rius, 2012)'
_computing_publication_material  'PLATON (Spek, 2003)'

#==============================================================================
# REFINEMENT


_pd_proc_ls_profile_function     Pseudo-Voigt
_pd_proc_ls_background_function  'Smoothing procedure (Br\~A1/4ckner, 2004)'
_pd_proc_ls_prof_wR_factor       0.067
_refine_ls_R_I_factor            0.079
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     1/Yobs
_refine_ls_hydrogen_treatment    noref
_refine_ls_number_reflns         1220
_refine_ls_number_parameters     76
_refine_ls_number_restraints     64
_refine_ls_goodness_of_fit_all   2.771
_refine_ls_shift/su_max          0.049
_refine_ls_shift/su_mean         0.031

_pd_proc_number_of_points        5416
_pd_proc_2theta_range_min        2.500
_pd_proc_2theta_range_max        35.000
_pd_proc_2theta_range_inc        0.006

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_Wyckoff_symbol
_atom_site_calc_flag
_atom_site_U_iso_or_equiv
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe01 FE 0.7511(5) 0.2500(9) 0.3582(4) 1.0000 4 e d 0.0613(11) . .
Cl1 CL 0.5998(20) 0.1200(8) 0.3033(4) 1.0000 4 e d 0.0565(5) . .
Cl2 CL 0.5925(20) 0.3744(8) 0.2903(4) 1.0000 4 e d 0.0565(5) . .
Cl3 CL 0.7419(7) 0.2552(17) 0.5174(4) 1.0000 4 e d 0.0565(5) . .
Cl4 CL 1.0626(6) 0.2506(13) 0.3155(4) 1.0000 4 e d 0.0565(5) . .
N11 N 1.1065(43) 0.4357(13) 0.5516(4) 0.5000 4 e d 0.0383(22) A -1
C12 C 1.0270(38) 0.4966(13) 0.4837(4) 0.5000 4 e d 0.0383(22) A -1
N13 N 0.8613(38) 0.5344(14) 0.5120(4) 0.5000 4 e d 0.0383(22) A -1
C14 C 0.8401(46) 0.4931(18) 0.6035(4) 0.5000 4 e d 0.0383(22) A -1
H14 H 0.7307 0.5098 0.6395 0.5000 4 e c 0.0383 A -1
C15 C 0.9875(53) 0.4317(16) 0.6310(4) 0.5000 4 e d 0.0383(22) A -1
H15 H 0.9997 0.3971 0.6905 0.5000 4 e c 0.0383 A -1
C16 C 1.2873(45) 0.3792(13) 0.5495(4) 0.5000 4 e d 0.0383(22) A -1
H16A H 1.3009 0.3432 0.6107 0.5000 4 e c 0.0383 A -1
H16B H 1.2743 0.3370 0.4929 0.5000 4 e c 0.0383 A -1
H16C H 1.4075 0.4178 0.5464 0.5000 4 e c 0.0383 A -1
C17 C 1.1156(45) 0.5172(16) 0.3908(4) 0.5000 4 e d 0.0383(22) A -1
H17A H 1.2358 0.4785 0.3908 0.5000 4 e c 0.0383 A -1
H17B H 1.0206 0.5014 0.3337 0.5000 4 e c 0.0383 A -1
H17C H 1.1535 0.5825 0.3870 0.5000 4 e c 0.0383 A -1
C18 C 0.7238(39) 0.6026(14) 0.4656(4) 0.5000 4 e d 0.0383(22) A -1
H18A H 0.6137 0.6178 0.5051 0.5000 4 e c 0.0383 A -1
H18B H 0.8022 0.6586 0.4552 0.5000 4 e c 0.0383 A -1
H18C H 0.6693 0.5777 0.4017 0.5000 4 e c 0.0383 A -1
N21 N 1.0700(79) 0.0284(18) 0.5245(4) 0.5000 4 e d 0.2039(45) B -1
C22 C 1.0200(62) -0.0211(17) 0.4431(4) 0.5000 4 e d 0.2039(45) B -1
N23 N 0.8515(62) -0.0685(18) 0.4554(4) 0.5000 4 e d 0.2039(45) B -1
C24 C 0.7916(79) -0.0485(26) 0.5486(4) 0.5000 4 e d 0.2039(45) B -1
H24 H 0.6843 -0.0676 0.5846 0.5000 4 e c 0.2039 B -1
C25 C 0.9282(94) 0.0124(26) 0.5922(4) 0.5000 4 e d 0.2039(45) B -1
H25 H 0.9464 0.0428 0.6541 0.5000 4 e c 0.2039 B -1
C26 C 1.2421(88) 0.0905(17) 0.5448(4) 0.5000 4 e d 0.2039(45) B -1
H26A H 1.2581 0.1213 0.6092 0.5000 4 e c 0.2039 B -1
H26B H 1.3612 0.0524 0.5371 0.5000 4 e c 0.2039 B -1
H26C H 1.2275 0.1372 0.4925 0.5000 4 e c 0.2039 B -1
C27 C 1.1291(63) -0.0237(22) 0.3551(4) 0.5000 4 e d 0.2039(45) B -1
H27A H 1.0460 -0.0667 0.3133 0.5000 4 e c 0.2039 B -1
H27B H 1.1324 0.0365 0.3221 0.5000 4 e c 0.2039 B -1
H27C H 1.2665 -0.0481 0.3666 0.5000 4 e c 0.2039 B -1
C28 C 0.7450(61) -0.1313(17) 0.3845(4) 0.5000 4 e d 0.2039(45) B -1
H28A H 0.6345 -0.1515 0.4219 0.5000 4 e c 0.2039 B -1
H28B H 0.6896 -0.0999 0.3241 0.5000 4 e c 0.2039 B -1
H28C H 0.8231 -0.1853 0.3673 0.5000 4 e c 0.2039 B -1


#===============================================================================
# MOLECULAR GEOMETRY

_geom_special_details            
;
 Bond distances, angles etc. have been calculated using the
 rounded fractional coordinates. All su's are estimated
 from the variances of the (full) variance-covariance matrix.
 The cell esds are taken into account in the estimation of
 distances, angles and torsion angles
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe01 Cl1 2.193(16) . . ?
Fe01 Cl2 2.206(15) . . ?
Fe01 Cl3 2.169(8) . . ?
Fe01 Cl4 2.198(5) . . ?
N11 C12 1.33(2) . . ?
N11 C15 1.40(3) . . ?
N11 C16 1.44(4) . . ?
N13 C12 1.32(3) . . ?
N13 C14 1.393(17) . . ?
N13 C18 1.43(3) . . ?
N21 C22 1.32(2) . . ?
N21 C25 1.40(6) . . ?
N21 C26 1.44(6) . . ?
N23 C22 1.33(5) . . ?
N23 C24 1.39(3) . . ?
N23 C28 1.44(3) . . ?
C12 C17 1.48(2) . . ?
C14 C15 1.34(4) . . ?
C22 C27 1.46(3) . . ?
C24 C25 1.34(6) . . ?
C14 H14 0.9400 . . ?
C15 H15 0.9400 . . ?
C16 H16A 0.9700 . . ?
C16 H16B 0.9700 . . ?
C16 H16C 0.9700 . . ?
C17 H17A 0.9600 . . ?
C17 H17B 0.9700 . . ?
C17 H17C 0.9600 . . ?
C18 H18A 0.9700 . . ?
C18 H18B 0.9700 . . ?
C18 H18C 0.9700 . . ?
C24 H24 0.9400 . . ?
C25 H25 0.9400 . . ?
C26 H26A 0.9700 . . ?
C26 H26B 0.9700 . . ?
C26 H26C 0.9700 . . ?
C27 H27A 0.9600 . . ?
C27 H27B 0.9700 . . ?
C27 H27C 0.9700 . . ?
C28 H28A 0.9800 . . ?
C28 H28B 0.9700 . . ?
C28 H28C 0.9700 . . ?

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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cl1 Fe01 Cl2 110.6(4) . . . ?
Cl1 Fe01 Cl3 108.0(7) . . . ?
Cl1 Fe01 Cl4 108.7(7) . . . ?
Cl2 Fe01 Cl3 109.2(7) . . . ?
Cl2 Fe01 Cl4 107.7(7) . . . ?
Cl3 Fe01 Cl4 112.7(3) . . . ?
C12 N11 C15 110(2) . . . ?
C12 N11 C16 128.2(16) . . . ?
C15 N11 C16 121.7(15) . . . ?
C12 N13 C14 104.6(19) . . . ?
C12 N13 C18 131.3(12) . . . ?
C14 N13 C18 124(2) . . . ?
C22 N21 C25 109(4) . . . ?
C22 N21 C26 128(3) . . . ?
C25 N21 C26 123(2) . . . ?
C22 N23 C24 110(3) . . . ?
C22 N23 C28 126.2(19) . . . ?
C24 N23 C28 124(3) . . . ?
N11 C12 N13 110.3(15) . . . ?
N11 C12 C17 124(2) . . . ?
N13 C12 C17 126.0(17) . . . ?
N13 C14 C15 113(2) . . . ?
N11 C15 C14 102.3(14) . . . ?
N21 C22 N23 108(3) . . . ?
N21 C22 C27 127(4) . . . ?
N23 C22 C27 125.5(19) . . . ?
N23 C24 C25 107(4) . . . ?
N21 C25 C24 106(2) . . . ?
N13 C14 H14 121.00 . . . ?
C15 C14 H14 127.00 . . . ?
N11 C15 H15 133.00 . . . ?
C14 C15 H15 125.00 . . . ?
N11 C16 H16A 106.00 . . . ?
N11 C16 H16B 111.00 . . . ?
N11 C16 H16C 112.00 . . . ?
H16A C16 H16B 110.00 . . . ?
H16A C16 H16C 109.00 . . . ?
H16B C16 H16C 109.00 . . . ?
C12 C17 H17A 107.00 . . . ?
C12 C17 H17B 111.00 . . . ?
C12 C17 H17C 111.00 . . . ?
H17A C17 H17B 110.00 . . . ?
H17A C17 H17C 109.00 . . . ?
H17B C17 H17C 109.00 . . . ?
N13 C18 H18A 113.00 . . . ?
N13 C18 H18B 107.00 . . . ?
N13 C18 H18C 108.00 . . . ?
H18A C18 H18B 110.00 . . . ?
H18A C18 H18C 110.00 . . . ?
H18B C18 H18C 109.00 . . . ?
N23 C24 H24 136.00 . . . ?
C25 C24 H24 117.00 . . . ?
N21 C25 H25 118.00 . . . ?
C24 C25 H25 135.00 . . . ?
N21 C26 H26A 117.00 . . . ?
N21 C26 H26B 106.00 . . . ?
N21 C26 H26C 105.00 . . . ?
H26A C26 H26B 109.00 . . . ?
H26A C26 H26C 110.00 . . . ?
H26B C26 H26C 109.00 . . . ?
C22 C27 H27A 102.00 . . . ?
C22 C27 H27B 113.00 . . . ?
C22 C27 H27C 114.00 . . . ?
H27A C27 H27B 109.00 . . . ?
H27A C27 H27C 110.00 . . . ?
H27B C27 H27C 109.00 . . . ?
N23 C28 H28A 100.00 . . . ?
N23 C28 H28B 113.00 . . . ?
N23 C28 H28C 114.00 . . . ?
H28A C28 H28B 110.00 . . . ?
H28A C28 H28C 110.00 . . . ?
H28B C28 H28C 109.00 . . . ?

