# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry C.
# 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_250K
_database_code_depnum_ccdc_archive 'CCDC 2003976'
loop_
_audit_author_name
_audit_author_address
'Garikoitz Beobide'
;Universidad del Pais Vasco
Spain
;
_audit_update_record             
;
2020-05-14 deposited with the CCDC.	2020-06-12 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3

_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C7 H14 Cl4 Fe N'
_chemical_formula_weight         309.85

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Fe Fe 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0000 0.0000 '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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'

_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+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'

_cell_length_a                   13.2030(10)
_cell_length_b                   12.8939(12)
_cell_length_c                   14.7769(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2515.6(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    250(2)
_cell_measurement_reflns_used    1453
_cell_measurement_theta_min      5.34
_cell_measurement_theta_max      55.65

_exptl_crystal_description       Prism
_exptl_crystal_colour            Yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.636
_exptl_crystal_F_000             410
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    0.259
_shelx_estimated_absorpt_T_min   0.975
_shelx_estimated_absorpt_T_max   0.975
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      250(2)
_diffrn_radiation_wavelength     1.45566
_diffrn_radiation_type           neutron
_diffrn_source                   'neutron source'
_diffrn_measurement_device_type  'D19, ILL'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            5482
_diffrn_reflns_av_unetI/netI     0.0362
_diffrn_reflns_av_R_equivalents  0.0447
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         5.337
_diffrn_reflns_theta_max         60.737
_diffrn_reflns_theta_full        60.737
_diffrn_measured_fraction_theta_max 0.769
_diffrn_measured_fraction_theta_full 0.768
_diffrn_reflns_Laue_measured_fraction_max 0.769
_diffrn_reflns_Laue_measured_fraction_full 0.768
_diffrn_reflns_point_group_measured_fraction_max 0.769
_diffrn_reflns_point_group_measured_fraction_full 0.768
_reflns_number_total             1743
_reflns_number_gt                1278
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1743
_refine_ls_number_parameters     244
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1001
_refine_ls_R_factor_gt           0.0775
_refine_ls_wR_factor_ref         0.2255
_refine_ls_wR_factor_gt          0.2114
_refine_ls_goodness_of_fit_ref   1.605
_refine_ls_restrained_S_all      1.605
_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 0.52749(15) 0.5368(2) 0.24779(10) 0.0488(7) Uani 1 1 d . . . . .
Cl1 Cl 0.68663(17) 0.4915(3) 0.24775(13) 0.0694(9) Uani 1 1 d . . . . .
N1 N 0.34046(19) 0.6938(2) 0.57705(15) 0.0626(8) Uani 1 1 d . . . . .
Cl2 Cl 0.46209(18) 0.4711(2) 0.37147(14) 0.0731(9) Uani 1 1 d . . . . .
Cl3 Cl 0.4537(2) 0.4786(2) 0.12641(14) 0.0731(9) Uani 1 1 d . . . . .
Cl4 Cl 0.5132(3) 0.7058(3) 0.24954(14) 0.0824(10) Uani 1 1 d . . . . .
C1 C 0.2270(3) 0.7737(4) 0.4593(2) 0.0780(14) Uani 1 1 d . . . . .
C2 C 0.3357(4) 0.8132(6) 0.4496(3) 0.0962(18) Uani 1 1 d . . . . .
C3 C 0.2286(4) 0.6554(5) 0.4516(3) 0.0898(15) Uani 1 1 d . . . . .
C4 C 0.2881(4) 0.6087(4) 0.5276(3) 0.0767(13) Uani 1 1 d . . . . .
C5 C 0.1894(5) 0.7993(7) 0.5552(3) 0.0965(19) Uani 1 1 d . . . . .
C6 C 0.4042(3) 0.7529(4) 0.5132(3) 0.0811(14) Uani 1 1 d . . . . .
C7 C 0.2650(3) 0.7609(4) 0.6231(2) 0.0744(13) Uani 1 1 d . . . . .
H1 H 0.3841(7) 0.6636(9) 0.6219(5) 0.101(3) Uani 1 1 d . . . . .
H2 H 0.2433(9) 0.5704(9) 0.5763(7) 0.107(3) Uani 1 1 d . . . . .
H3 H 0.2292(9) 0.7156(9) 0.6726(6) 0.121(4) Uani 1 1 d . . . . .
H4 H 0.2652(14) 0.6365(11) 0.3868(8) 0.155(6) Uani 1 1 d . . . . .
H5 H 0.3600(11) 0.8072(13) 0.3815(7) 0.166(6) Uani 1 1 d . . . . .
H6 H 0.4473(8) 0.8051(12) 0.5523(8) 0.140(5) Uani 1 1 d . . . . .
H7 H 0.3400(11) 0.5610(9) 0.5046(8) 0.116(4) Uani 1 1 d . . . . .
H8 H 0.3061(8) 0.8229(11) 0.6542(7) 0.125(4) Uani 1 1 d . . . . .
H9 H 0.1772(10) 0.8055(11) 0.4093(7) 0.143(5) Uani 1 1 d . . . . .
H10 H 0.4505(7) 0.7006(11) 0.4785(7) 0.122(4) Uani 1 1 d . . . . .
H11 H 0.1679(14) 0.8735(13) 0.5618(8) 0.159(8) Uani 1 1 d . . . . .
H12 H 0.1550(11) 0.6224(13) 0.4495(10) 0.172(7) Uani 1 1 d . . . . .
H13 H 0.3398(15) 0.8927(14) 0.4669(11) 0.164(7) Uani 1 1 d . . . . .
H14 H 0.1218(9) 0.7565(12) 0.5674(7) 0.123(4) Uani 1 1 d . . . . .


_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 Cl3 2.175(3) . ?
Fe1 Cl1 2.181(3) . ?
Fe1 Cl4 2.186(5) . ?
Fe1 Cl2 2.192(3) . ?
N1 C6 1.476(5) . ?
N1 C7 1.485(5) . ?
N1 C4 1.489(6) . ?
N1 H1 0.961(10) . ?
C1 C2 1.529(7) . ?
C1 C3 1.529(8) . ?
C1 C5 1.537(6) . ?
C1 H9 1.071(9) . ?
C2 C6 1.519(7) . ?
C2 H5 1.059(12) . ?
C2 H13 1.06(2) . ?
C3 C4 1.496(7) . ?
C3 H4 1.100(15) . ?
C3 H12 1.060(14) . ?
C4 H2 1.055(12) . ?
C4 H7 0.982(16) . ?
C5 C7 1.499(6) . ?
C5 H11 1.003(19) . ?
C5 H14 1.065(18) . ?
C6 H6 1.053(13) . ?
C6 H10 1.046(14) . ?
C7 H3 1.048(12) . ?
C7 H8 1.071(15) . ?

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
Cl3 Fe1 Cl1 109.82(13) . . ?
Cl3 Fe1 Cl4 108.35(14) . . ?
Cl1 Fe1 Cl4 110.50(17) . . ?
Cl3 Fe1 Cl2 112.18(17) . . ?
Cl1 Fe1 Cl2 106.02(12) . . ?
Cl4 Fe1 Cl2 109.97(14) . . ?
C6 N1 C7 112.0(4) . . ?
C6 N1 C4 109.4(3) . . ?
C7 N1 C4 110.0(3) . . ?
C6 N1 H1 108.0(7) . . ?
C7 N1 H1 108.7(6) . . ?
C4 N1 H1 108.6(7) . . ?
C2 C1 C3 108.2(4) . . ?
C2 C1 C5 108.6(4) . . ?
C3 C1 C5 106.7(4) . . ?
C2 C1 H9 112.6(9) . . ?
C3 C1 H9 109.8(9) . . ?
C5 C1 H9 110.8(7) . . ?
C6 C2 C1 109.3(4) . . ?
C6 C2 H5 111.8(10) . . ?
C1 C2 H5 110.5(11) . . ?
C6 C2 H13 108.4(10) . . ?
C1 C2 H13 110.4(11) . . ?
H5 C2 H13 106.5(12) . . ?
C4 C3 C1 110.6(4) . . ?
C4 C3 H4 109.4(9) . . ?
C1 C3 H4 107.0(9) . . ?
C4 C3 H12 110.0(9) . . ?
C1 C3 H12 112.9(10) . . ?
H4 C3 H12 106.7(11) . . ?
N1 C4 C3 108.4(4) . . ?
N1 C4 H2 105.7(7) . . ?
C3 C4 H2 114.0(8) . . ?
N1 C4 H7 107.8(8) . . ?
C3 C4 H7 111.1(8) . . ?
H2 C4 H7 109.5(11) . . ?
C7 C5 C1 109.4(4) . . ?
C7 C5 H11 116.0(10) . . ?
C1 C5 H11 112.7(8) . . ?
C7 C5 H14 105.9(8) . . ?
C1 C5 H14 108.4(7) . . ?
H11 C5 H14 103.8(12) . . ?
N1 C6 C2 108.7(4) . . ?
N1 C6 H6 106.7(7) . . ?
C2 C6 H6 109.5(9) . . ?
N1 C6 H10 108.3(7) . . ?
C2 C6 H10 112.0(7) . . ?
H6 C6 H10 111.4(10) . . ?
N1 C7 C5 109.4(3) . . ?
N1 C7 H3 107.3(7) . . ?
C5 C7 H3 110.6(8) . . ?
N1 C7 H8 106.9(6) . . ?
C5 C7 H8 112.2(9) . . ?
H3 C7 H8 110.3(10) . . ?

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
C3 C1 C2 C6 -50.1(5) . . . . ?
C5 C1 C2 C6 65.3(6) . . . . ?
C2 C1 C3 C4 63.4(5) . . . . ?
C5 C1 C3 C4 -53.2(5) . . . . ?
C6 N1 C4 C3 -56.6(5) . . . . ?
C7 N1 C4 C3 66.8(5) . . . . ?
C1 C3 C4 N1 -9.3(5) . . . . ?
C2 C1 C5 C7 -51.5(7) . . . . ?
C3 C1 C5 C7 64.9(7) . . . . ?
C7 N1 C6 C2 -52.6(5) . . . . ?
C4 N1 C6 C2 69.7(5) . . . . ?
C1 C2 C6 N1 -12.6(6) . . . . ?
C6 N1 C7 C5 66.9(6) . . . . ?
C4 N1 C7 C5 -55.0(6) . . . . ?
C1 C5 C7 N1 -10.7(8) . . . . ?

_refine_diff_density_max         0.546
_refine_diff_density_min         -0.695
_refine_diff_density_rms         0.131



####################################################################### 
# 
# 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_shelx
_database_code_depnum_ccdc_archive 'CCDC 2003979'
loop_
_audit_author_name
_audit_author_address
'Garikoitz Beobide'
;Universidad del Pais Vasco
Spain
;
_audit_update_record             
;
2020-05-14 deposited with the CCDC.	2020-06-12 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7

_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C7 H14 Cl4 Fe N'
_chemical_formula_weight         309.84

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      Orthorhombic
_space_group_IT_number           29
_space_group_name_H-M_alt        'P b c 21'
_space_group_name_Hall           'P 2c -2b'

_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, z+1/2'
'-x, y+1/2, z'
'x, -y+1/2, z+1/2'

_cell_length_a                   6.6991(2)
_cell_length_b                   13.1984(5)
_cell_length_c                   14.6266(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1293.25(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    300(2)
_cell_measurement_reflns_used    3507
_cell_measurement_theta_min      3.3690
_cell_measurement_theta_max      25.0270

_exptl_crystal_description       Prism
_exptl_crystal_colour            Yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.591
_exptl_crystal_F_000             628
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.11
_exptl_absorpt_coefficient_mu    1.952
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_T_min  0.50251
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.722
_oxdiff_exptl_absorpt_empirical_full_max 1.542
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_diffrn_ambient_temperature      300(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            8183
_diffrn_reflns_av_unetI/netI     0.0196
_diffrn_reflns_av_R_equivalents  0.0210
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.785
_diffrn_reflns_theta_max         27.409
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.944
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.944
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.945
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             2619
_reflns_number_gt                2069
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.922
_reflns_Friedel_fraction_max     0.945
_reflns_Friedel_fraction_full    1.000

_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
  Refined as a 2-component merohedral twin, implying that the compound crystallizes in a unit cell with a higher point group than that corresponding to the Pbc21. The resoluction in Pbcm space group yields greater R1 and wR2 factors and a highly disorded organic cation tangled to be modeled unambiguously
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0938P)²+1.1100P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.47(7)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         2619
_refine_ls_number_parameters     118
_refine_ls_number_restraints     33
_refine_ls_R_factor_all          0.0679
_refine_ls_R_factor_gt           0.0545
_refine_ls_wR_factor_ref         0.1736
_refine_ls_wR_factor_gt          0.1580
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_restrained_S_all      1.073
_refine_ls_shift/su_max          0.020
_refine_ls_shift/su_mean         0.004

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 -0.06195(12) 0.03569(7) 0.44061(18) 0.0580(4) Uani 1 1 d . . . . .
Cl1 Cl 0.0730(7) -0.0253(3) 0.5638(2) 0.0957(16) Uani 1 1 d . . . . .
Cl4 Cl 0.0750(7) -0.0257(4) 0.3165(3) 0.1064(18) Uani 1 1 d . . . . .
Cl2 Cl -0.3782(3) -0.0052(2) 0.4402(5) 0.0973(7) Uani 1 1 d . . . . .
Cl3 Cl -0.0295(4) 0.20067(15) 0.4397(5) 0.1039(8) Uani 1 1 d . . . . .
N1A N 0.332(3) 0.2072(15) 0.1285(13) 0.25(2) Uiso 0.663(18) 1 d D . P A 1
H1A H 0.256(3) 0.1794(18) 0.0893(14) 0.301 Uiso 0.663(18) 1 d D U P A 1
C2A C 0.448(2) 0.1213(11) 0.1695(12) 0.077(4) Uiso 0.663(18) 1 d D . P A 1
H2A1 H 0.5112 0.0801 0.1230 0.092 Uiso 0.663(18) 1 calc R U P A 1
H2A2 H 0.3637 0.0788 0.2076 0.092 Uiso 0.663(18) 1 calc R U P A 1
C7A C 0.333(2) 0.3032(13) 0.2622(12) 0.071(5) Uiso 0.663(18) 1 d D . P A 1
H7A1 H 0.3090 0.2823 0.3248 0.085 Uiso 0.663(18) 1 calc R U P A 1
H7A2 H 0.2976 0.3742 0.2577 0.085 Uiso 0.663(18) 1 calc R U P A 1
C8A C 0.1968(18) 0.2449(15) 0.2020(11) 0.074(4) Uiso 0.663(18) 1 d D . P A 1
H8A1 H 0.0929 0.2880 0.1771 0.089 Uiso 0.663(18) 1 calc R U P A 1
H8A2 H 0.1356 0.1891 0.2348 0.089 Uiso 0.663(18) 1 calc R U P A 1
C4A C 0.558(3) 0.2932(19) 0.243(2) 0.40(5) Uiso 0.663(18) 1 d D . P A 1
H4A H 0.6457 0.3262 0.2878 0.482 Uiso 0.663(18) 1 calc R U P A 1
C5A C 0.552(3) 0.3436(19) 0.1486(13) 0.101(7) Uiso 0.663(18) 1 d D . P A 1
H5A1 H 0.4727 0.4049 0.1526 0.121 Uiso 0.663(18) 1 calc R U P A 1
H5A2 H 0.6865 0.3630 0.1313 0.121 Uiso 0.663(18) 1 calc R U P A 1
C3A C 0.601(3) 0.1801(16) 0.2265(14) 0.096(6) Uiso 0.663(18) 1 d D . P A 1
H3A1 H 0.7299 0.1745 0.1964 0.115 Uiso 0.663(18) 1 calc R U P A 1
H3A2 H 0.6132 0.1471 0.2855 0.115 Uiso 0.663(18) 1 calc R U P A 1
C6A C 0.465(3) 0.2758(15) 0.0744(11) 0.088(5) Uiso 0.663(18) 1 d D . P A 1
H6A1 H 0.3900 0.3147 0.0299 0.105 Uiso 0.663(18) 1 calc R U P A 1
H6A2 H 0.5691 0.2379 0.0431 0.105 Uiso 0.663(18) 1 calc R U P A 1
N1B N 0.319(3) 0.2105(15) 0.1238(14) 0.062(8) Uiso 0.337(18) 1 d D . P A 2
H1B H 0.233(4) 0.193(3) 0.0845(19) 0.074 Uiso 0.337(18) 1 d D U P A 2
C2B C 0.342(8) 0.124(2) 0.188(3) 0.18(3) Uiso 0.337(18) 1 d D . P A 2
H2B1 H 0.4112 0.0678 0.1597 0.216 Uiso 0.337(18) 1 calc R U P A 2
H2B2 H 0.2144 0.1016 0.2116 0.216 Uiso 0.337(18) 1 calc R U P A 2
C7B C 0.373(5) 0.356(3) 0.236(3) 0.15(2) Uiso 0.337(18) 1 d D . P A 2
H7B1 H 0.3102 0.3625 0.2956 0.180 Uiso 0.337(18) 1 calc R U P A 2
H7B2 H 0.4147 0.4220 0.2148 0.180 Uiso 0.337(18) 1 calc R U P A 2
C8B C 0.235(5) 0.304(2) 0.168(2) 0.110(12) Uiso 0.337(18) 1 d D . P A 2
H8B1 H 0.1124 0.2862 0.1988 0.132 Uiso 0.337(18) 1 calc R U P A 2
H8B2 H 0.2023 0.3524 0.1202 0.132 Uiso 0.337(18) 1 calc R U P A 2
C4B C 0.551(3) 0.2815(14) 0.2400(12) 0.049(6) Uiso 0.337(18) 1 d D . P A 2
H4B H 0.6507 0.3028 0.2853 0.059 Uiso 0.337(18) 1 calc R U P A 2
C5B C 0.639(4) 0.279(3) 0.1428(13) 0.081(9) Uiso 0.337(18) 1 d D . P A 2
H5B1 H 0.6713 0.3483 0.1249 0.097 Uiso 0.337(18) 1 calc R U P A 2
H5B2 H 0.7633 0.2414 0.1443 0.097 Uiso 0.337(18) 1 calc R U P A 2
C3B C 0.469(7) 0.176(2) 0.261(3) 0.142(18) Uiso 0.337(18) 1 d D . P A 2
H3B1 H 0.5807 0.1316 0.2750 0.170 Uiso 0.337(18) 1 calc R U P A 2
H3B2 H 0.3887 0.1805 0.3165 0.170 Uiso 0.337(18) 1 calc R U P A 2
C6B C 0.505(4) 0.233(3) 0.0704(19) 0.118(16) Uiso 0.337(18) 1 d D . P A 2
H6B1 H 0.4782 0.2811 0.0215 0.141 Uiso 0.337(18) 1 calc R U P A 2
H6B2 H 0.5625 0.1723 0.0449 0.141 Uiso 0.337(18) 1 calc R U P A 2


_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 Cl1 2.171(4) . ?
Fe1 Cl2 2.186(2) . ?
Fe1 Cl3 2.188(2) . ?
Fe1 Cl4 2.189(5) . ?
N1A C8A 1.493(13) . ?
N1A C6A 1.496(12) . ?
N1A C2A 1.497(13) . ?
N1A H1A 0.852(13) . ?
C2A C3A 1.536(12) . ?
C2A H2A1 0.9700 . ?
C2A H2A2 0.9700 . ?
C7A C8A 1.483(12) . ?
C7A C4A 1.541(14) . ?
C7A H7A1 0.9700 . ?
C7A H7A2 0.9700 . ?
C8A H8A1 0.9700 . ?
C8A H8A2 0.9700 . ?
C4A C5A 1.534(14) . ?
C4A C3A 1.539(14) . ?
C4A H4A 0.9800 . ?
C5A C6A 1.523(13) . ?
C5A H5A1 0.9700 . ?
C5A H5A2 0.9700 . ?
C3A H3A1 0.9700 . ?
C3A H3A2 0.9700 . ?
C6A H6A1 0.9700 . ?
C6A H6A2 0.9700 . ?
N1B C2B 1.481(12) . ?
N1B C6B 1.498(12) . ?
N1B C8B 1.501(12) . ?
N1B H1B 0.847(12) . ?
C2B C3B 1.529(14) . ?
C2B H2B1 0.9700 . ?
C2B H2B2 0.9700 . ?
C7B C8B 1.523(14) . ?
C7B C4B 1.542(13) . ?
C7B H7B1 0.9700 . ?
C7B H7B2 0.9700 . ?
C8B H8B1 0.9700 . ?
C8B H8B2 0.9700 . ?
C4B C3B 1.535(13) . ?
C4B C5B 1.540(13) . ?
C4B H4B 0.9800 . ?
C5B C6B 1.518(14) . ?
C5B H5B1 0.9700 . ?
C5B H5B2 0.9700 . ?
C3B H3B1 0.9700 . ?
C3B H3B2 0.9700 . ?
C6B H6B1 0.9700 . ?
C6B H6B2 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_3
_geom_angle_publ_flag
Cl1 Fe1 Cl2 108.3(2) . . ?
Cl1 Fe1 Cl3 109.4(2) . . ?
Cl2 Fe1 Cl3 109.99(11) . . ?
Cl1 Fe1 Cl4 112.14(12) . . ?
Cl2 Fe1 Cl4 108.2(2) . . ?
Cl3 Fe1 Cl4 108.7(2) . . ?
C8A N1A C6A 122.8(16) . . ?
C8A N1A C2A 106.1(15) . . ?
C6A N1A C2A 111.3(16) . . ?
C8A N1A H1A 105.2(16) . . ?
C6A N1A H1A 105.3(15) . . ?
C2A N1A H1A 104.7(16) . . ?
N1A C2A C3A 100.4(14) . . ?
N1A C2A H2A1 111.7 . . ?
C3A C2A H2A1 111.7 . . ?
N1A C2A H2A2 111.7 . . ?
C3A C2A H2A2 111.7 . . ?
H2A1 C2A H2A2 109.5 . . ?
C8A C7A C4A 116.8(17) . . ?
C8A C7A H7A1 108.1 . . ?
C4A C7A H7A1 108.1 . . ?
C8A C7A H7A2 108.1 . . ?
C4A C7A H7A2 108.1 . . ?
H7A1 C7A H7A2 107.3 . . ?
C7A C8A N1A 103.1(13) . . ?
C7A C8A H8A1 111.1 . . ?
N1A C8A H8A1 111.2 . . ?
C7A C8A H8A2 111.2 . . ?
N1A C8A H8A2 111.1 . . ?
H8A1 C8A H8A2 109.1 . . ?
C5A C4A C3A 107(2) . . ?
C5A C4A C7A 95.7(18) . . ?
C3A C4A C7A 107.1(19) . . ?
C5A C4A H4A 115.2 . . ?
C3A C4A H4A 115.2 . . ?
C7A C4A H4A 115.2 . . ?
C6A C5A C4A 113.4(19) . . ?
C6A C5A H5A1 108.9 . . ?
C4A C5A H5A1 108.9 . . ?
C6A C5A H5A2 108.9 . . ?
C4A C5A H5A2 108.9 . . ?
H5A1 C5A H5A2 107.7 . . ?
C2A C3A C4A 116.7(18) . . ?
C2A C3A H3A1 108.1 . . ?
C4A C3A H3A1 108.1 . . ?
C2A C3A H3A2 108.1 . . ?
C4A C3A H3A2 108.1 . . ?
H3A1 C3A H3A2 107.3 . . ?
N1A C6A C5A 101.9(16) . . ?
N1A C6A H6A1 111.4 . . ?
C5A C6A H6A1 111.4 . . ?
N1A C6A H6A2 111.4 . . ?
C5A C6A H6A2 111.4 . . ?
H6A1 C6A H6A2 109.3 . . ?
C2B N1B C6B 113.5(11) . . ?
C2B N1B C8B 113.6(11) . . ?
C6B N1B C8B 111.6(11) . . ?
C2B N1B H1B 107.0(15) . . ?
C6B N1B H1B 105.4(15) . . ?
C8B N1B H1B 105.0(15) . . ?
N1B C2B C3B 99(2) . . ?
N1B C2B H2B1 111.9 . . ?
C3B C2B H2B1 111.9 . . ?
N1B C2B H2B2 111.9 . . ?
C3B C2B H2B2 111.9 . . ?
H2B1 C2B H2B2 109.6 . . ?
C8B C7B C4B 102(2) . . ?
C8B C7B H7B1 111.3 . . ?
C4B C7B H7B1 111.3 . . ?
C8B C7B H7B2 111.4 . . ?
C4B C7B H7B2 111.4 . . ?
H7B1 C7B H7B2 109.2 . . ?
N1B C8B C7B 115(2) . . ?
N1B C8B H8B1 108.5 . . ?
C7B C8B H8B1 108.5 . . ?
N1B C8B H8B2 108.5 . . ?
C7B C8B H8B2 108.5 . . ?
H8B1 C8B H8B2 107.5 . . ?
C3B C4B C5B 108.0(12) . . ?
C3B C4B C7B 107.8(12) . . ?
C5B C4B C7B 105.9(11) . . ?
C3B C4B H4B 111.6 . . ?
C5B C4B H4B 111.6 . . ?
C7B C4B H4B 111.6 . . ?
C6B C5B C4B 115(2) . . ?
C6B C5B H5B1 108.5 . . ?
C4B C5B H5B1 108.5 . . ?
C6B C5B H5B2 108.5 . . ?
C4B C5B H5B2 108.5 . . ?
H5B1 C5B H5B2 107.5 . . ?
C2B C3B C4B 117(2) . . ?
C2B C3B H3B1 107.9 . . ?
C4B C3B H3B1 107.9 . . ?
C2B C3B H3B2 108.0 . . ?
C4B C3B H3B2 108.0 . . ?
H3B1 C3B H3B2 107.2 . . ?
N1B C6B C5B 102.1(19) . . ?
N1B C6B H6B1 111.3 . . ?
C5B C6B H6B1 111.4 . . ?
N1B C6B H6B2 111.4 . . ?
C5B C6B H6B2 111.3 . . ?
H6B1 C6B H6B2 109.2 . . ?

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
C8A N1A C2A C3A -77.7(17) . . . . ?
C6A N1A C2A C3A 58.2(18) . . . . ?
C4A C7A C8A N1A -10(2) . . . . ?
C6A N1A C8A C7A -53(2) . . . . ?
C2A N1A C8A C7A 76.1(16) . . . . ?
C8A C7A C4A C5A 65.3(19) . . . . ?
C8A C7A C4A C3A -44(2) . . . . ?
C3A C4A C5A C6A 35(2) . . . . ?
C7A C4A C5A C6A -75(2) . . . . ?
N1A C2A C3A C4A 15(2) . . . . ?
C5A C4A C3A C2A -61(2) . . . . ?
C7A C4A C3A C2A 41(3) . . . . ?
C8A N1A C6A C5A 44(2) . . . . ?
C2A N1A C6A C5A -83(2) . . . . ?
C4A C5A C6A N1A 26(2) . . . . ?
C6B N1B C2B C3B 74(3) . . . . ?
C8B N1B C2B C3B -55(3) . . . . ?
C2B N1B C8B C7B 69(3) . . . . ?
C6B N1B C8B C7B -61(3) . . . . ?
C4B C7B C8B N1B -5(4) . . . . ?
C8B C7B C4B C3B -53(3) . . . . ?
C8B C7B C4B C5B 62(3) . . . . ?
C3B C4B C5B C6B 49(3) . . . . ?
C7B C4B C5B C6B -67(3) . . . . ?
N1B C2B C3B C4B -9(4) . . . . ?
C5B C4B C3B C2B -46(3) . . . . ?
C7B C4B C3B C2B 68(3) . . . . ?
C2B N1B C6B C5B -72(3) . . . . ?
C8B N1B C6B C5B 58(3) . . . . ?
C4B C5B C6B N1B 3(3) . . . . ?

_refine_diff_density_max         0.571
_refine_diff_density_min         -0.384
_refine_diff_density_rms         0.082



####################################################################### 
# 
# 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_shelx_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 2003977'
loop_
_audit_author_name
_audit_author_address
'Garikoitz Beobide'
;Universidad del Pais Vasco
Spain
;
_audit_update_record             
;
2020-05-14 deposited with the CCDC.	2020-06-12 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3

_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C7 H14 Cl4 Fe N'
_chemical_formula_weight         309.85

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0000 0.0000 '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 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      Orthorhombic
_space_group_IT_number           29
_space_group_name_H-M_alt        'P b c 21'
_space_group_name_Hall           'P 2c -2b'

_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, z+1/2'
'-x, y+1/2, z'
'x, -y+1/2, z+1/2'

_cell_length_a                   6.6726(19)
_cell_length_b                   13.1429(8)
_cell_length_c                   14.6275(15)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1282.8(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    782
_cell_measurement_theta_min      5.71
_cell_measurement_theta_max      55.75

_exptl_crystal_description       Prism
_exptl_crystal_colour            Yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.604
_exptl_crystal_F_000             205
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          2.200
_exptl_crystal_size_mid          2.100
_exptl_crystal_size_min          2.000
_exptl_absorpt_coefficient_mu    0.254
_shelx_estimated_absorpt_T_min   0.605
_shelx_estimated_absorpt_T_max   0.631
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      295(2)
_diffrn_radiation_wavelength     1.45566
_diffrn_radiation_type           neutron
_diffrn_source                   'neutron source'
_diffrn_measurement_device_type  'D19, ILL'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            2686
_diffrn_reflns_av_unetI/netI     0.0410
_diffrn_reflns_av_R_equivalents  0.0451
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         5.711
_diffrn_reflns_theta_max         60.646
_diffrn_reflns_theta_full        60.646
_diffrn_measured_fraction_theta_max 0.747
_diffrn_measured_fraction_theta_full 0.747
_diffrn_reflns_Laue_measured_fraction_max 0.747
_diffrn_reflns_Laue_measured_fraction_full 0.747
_diffrn_reflns_point_group_measured_fraction_max 0.415
_diffrn_reflns_point_group_measured_fraction_full 0.415
_reflns_number_total             957
_reflns_number_gt                643
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.065
_reflns_Friedel_fraction_max     0.053
_reflns_Friedel_fraction_full    0.053

_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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    refU
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 
;
 All f" are zero, so absolute structure could not be determined
;
_refine_ls_abs_structure_Flack   ?
_chemical_absolute_configuration ?
_refine_ls_number_reflns         957
_refine_ls_number_parameters     118
_refine_ls_number_restraints     41
_refine_ls_R_factor_all          0.2464
_refine_ls_R_factor_gt           0.2046
_refine_ls_wR_factor_ref         0.5602
_refine_ls_wR_factor_gt          0.5063
_refine_ls_goodness_of_fit_ref   2.485
_refine_ls_restrained_S_all      2.655
_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 -0.0607(10) 0.0353(7) 0.4415(8) 0.058(2) Uani 1 1 d . . . . .
Cl1 Cl 0.078(2) -0.0308(13) 0.5649(9) 0.098(5) Uani 1 1 d . . . . .
Cl4 Cl 0.071(2) -0.0243(15) 0.3195(11) 0.103(5) Uani 1 1 d . . . . .
Cl2 Cl -0.3744(14) -0.0084(11) 0.4470(10) 0.096(4) Uani 1 1 d . . . . .
Cl3 Cl -0.032(3) 0.2034(13) 0.4400(11) 0.120(5) Uani 1 1 d . . . . .
N1A N 0.324(3) 0.2106(19) 0.1269(13) 0.114(8) Uani 0.52(5) 1 d D . P A 1
C2A C 0.465(4) 0.127(2) 0.152(2) 0.114(8) Uani 0.52(5) 1 d D . P A 1
H2A1 H 0.537325 0.102756 0.099095 0.25(3) Uiso 0.52(5) 1 calc R . P A 1
H2A2 H 0.392137 0.070034 0.178957 0.25(3) Uiso 0.52(5) 1 calc R . P A 1
C7A C 0.332(4) 0.287(3) 0.272(2) 0.114(8) Uani 0.52(5) 1 d D . P A 1
H7A1 H 0.319509 0.250597 0.329497 0.25(3) Uiso 0.52(5) 1 calc R . P A 1
H7A2 H 0.293738 0.357235 0.283270 0.25(3) Uiso 0.52(5) 1 calc R . P A 1
C8A C 0.187(4) 0.241(3) 0.203(2) 0.114(8) Uani 0.52(5) 1 d D . P A 1
H8A1 H 0.118292 0.182470 0.228313 0.25(3) Uiso 0.52(5) 1 calc R . P A 1
H8A2 H 0.089324 0.290554 0.182701 0.25(3) Uiso 0.52(5) 1 calc R . P A 1
C4A C 0.554(4) 0.285(2) 0.2422(14) 0.114(8) Uani 0.52(5) 1 d D . P A 1
H4A H 0.641268 0.313639 0.289545 0.25(3) Uiso 0.52(5) 1 calc R . P A 1
C5A C 0.571(5) 0.345(3) 0.152(2) 0.114(8) Uani 0.52(5) 1 d D . P A 1
H5A1 H 0.538460 0.415739 0.162920 0.25(3) Uiso 0.52(5) 1 calc R . P A 1
H5A2 H 0.707401 0.341043 0.129433 0.25(3) Uiso 0.52(5) 1 calc R . P A 1
C3A C 0.608(5) 0.174(2) 0.222(2) 0.114(8) Uani 0.52(5) 1 d D . P A 1
H3A1 H 0.744364 0.170146 0.198861 0.138(19) Uiso 0.52(5) 1 calc R . P A 1
H3A2 H 0.603173 0.134621 0.278527 0.138(19) Uiso 0.52(5) 1 calc R . P A 1
C6A C 0.427(5) 0.299(2) 0.084(2) 0.114(8) Uani 0.52(5) 1 d D . P A 1
H6A1 H 0.329591 0.349688 0.065010 0.138(19) Uiso 0.52(5) 1 calc R . P A 1
H6A2 H 0.500157 0.276987 0.029750 0.138(19) Uiso 0.52(5) 1 calc R . P A 1
N1B N 0.335(3) 0.194(2) 0.1232(12) 0.113(8) Uani 0.48(5) 1 d D . P A 2
C2B C 0.422(5) 0.105(2) 0.1723(18) 0.113(8) Uani 0.48(5) 1 d D . P A 2
H2B1 H 0.511969 0.066470 0.133364 0.140(17) Uiso 0.48(5) 1 calc R . P A 2
H2B2 H 0.318720 0.060348 0.195907 0.140(17) Uiso 0.48(5) 1 calc R . P A 2
C7B C 0.335(4) 0.317(2) 0.248(2) 0.113(8) Uani 0.48(5) 1 d D . P A 2
H7B1 H 0.285407 0.311166 0.310197 0.140(17) Uiso 0.48(5) 1 calc R . P A 2
H7B2 H 0.333779 0.388939 0.231439 0.140(17) Uiso 0.48(5) 1 calc R . P A 2
C8B C 0.201(4) 0.257(2) 0.1828(18) 0.113(8) Uani 0.48(5) 1 d D . P A 2
H8B1 H 0.110359 0.213598 0.217068 0.140(17) Uiso 0.48(5) 1 calc R . P A 2
H8B2 H 0.121170 0.303029 0.145631 0.151(16) Uiso 0.48(5) 1 calc R . P A 2
C4B C 0.549(3) 0.274(2) 0.2412(14) 0.113(8) Uani 0.48(5) 1 d D . P A 2
H4B H 0.635058 0.302764 0.289150 0.151(16) Uiso 0.48(5) 1 calc R . P A 2
C5B C 0.631(5) 0.300(3) 0.1459(16) 0.113(8) Uani 0.48(5) 1 d D . P A 2
H5B1 H 0.640709 0.373366 0.138603 0.151(16) Uiso 0.48(5) 1 calc R . P A 2
H5B2 H 0.763665 0.271248 0.138379 0.151(16) Uiso 0.48(5) 1 calc R . P A 2
C3B C 0.535(5) 0.1582(19) 0.2492(19) 0.113(8) Uani 0.48(5) 1 d D . P A 2
H3B1 H 0.670083 0.130818 0.251532 0.151(16) Uiso 0.48(5) 1 calc R . P A 2
H3B2 H 0.470304 0.141632 0.306620 0.151(16) Uiso 0.48(5) 1 calc R . P A 2
C6B C 0.489(5) 0.256(3) 0.0745(17) 0.113(8) Uani 0.48(5) 1 d D . P A 2
H6B1 H 0.424892 0.310880 0.040729 0.151(16) Uiso 0.48(5) 1 calc R . P A 2
H6B2 H 0.562762 0.214255 0.031614 0.151(16) Uiso 0.48(5) 1 calc R . P A 2
H1A H 0.249(5) 0.186(3) 0.0856(19) 0.138(19) Uiso 0.52(5) 1 d D . P A 1
H1B H 0.260(4) 0.170(3) 0.0820(15) 0.140(17) Uiso 0.48(5) 1 d D . P A 2


_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 Cl4 2.137(14) . ?
Fe1 Cl2 2.172(11) . ?
Fe1 Cl1 2.206(12) . ?
Fe1 Cl3 2.22(2) . ?
N1A C8A 1.493(10) . ?
N1A C6A 1.493(9) . ?
N1A C2A 1.495(9) . ?
N1A H1A 0.850(9) . ?
C2A C3A 1.531(11) . ?
C2A H2A1 0.9700 . ?
C2A H2A2 0.9700 . ?
C7A C8A 1.526(11) . ?
C7A C4A 1.543(10) . ?
C7A H7A1 0.9700 . ?
C7A H7A2 0.9700 . ?
C8A H8A1 0.9700 . ?
C8A H8A2 0.9700 . ?
C4A C5A 1.535(10) . ?
C4A C3A 1.536(10) . ?
C4A H4A 0.9800 . ?
C5A C6A 1.516(11) . ?
C5A H5A1 0.9700 . ?
C5A H5A2 0.9700 . ?
C3A H3A1 0.9700 . ?
C3A H3A2 0.9700 . ?
C6A H6A1 0.9700 . ?
C6A H6A2 0.9700 . ?
N1B C2B 1.490(10) . ?
N1B C6B 1.496(10) . ?
N1B C8B 1.500(9) . ?
N1B H1B 0.845(9) . ?
C2B C3B 1.523(11) . ?
C2B H2B1 0.9700 . ?
C2B H2B2 0.9700 . ?
C7B C8B 1.530(11) . ?
C7B C4B 1.542(10) . ?
C7B H7B1 0.9700 . ?
C7B H7B2 0.9700 . ?
C8B H8B1 0.9700 . ?
C8B H8B2 0.9700 . ?
C4B C5B 1.535(10) . ?
C4B C3B 1.536(10) . ?
C4B H4B 0.9800 . ?
C5B C6B 1.523(11) . ?
C5B H5B1 0.9700 . ?
C5B H5B2 0.9700 . ?
C3B H3B1 0.9700 . ?
C3B H3B2 0.9700 . ?
C6B H6B1 0.9700 . ?
C6B H6B2 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_3
_geom_angle_publ_flag
Cl4 Fe1 Cl2 109.3(7) . . ?
Cl4 Fe1 Cl1 111.5(6) . . ?
Cl2 Fe1 Cl1 105.6(7) . . ?
Cl4 Fe1 Cl3 108.7(8) . . ?
Cl2 Fe1 Cl3 110.3(7) . . ?
Cl1 Fe1 Cl3 111.3(7) . . ?
C8A N1A C6A 113.0(9) . . ?
C8A N1A C2A 113.2(9) . . ?
C6A N1A C2A 113.0(9) . . ?
C8A N1A H1A 105.6(12) . . ?
C6A N1A H1A 105.6(11) . . ?
C2A N1A H1A 105.6(12) . . ?
N1A C2A C3A 105.3(18) . . ?
N1A C2A H2A1 110.7 . . ?
C3A C2A H2A1 110.7 . . ?
N1A C2A H2A2 110.7 . . ?
C3A C2A H2A2 110.7 . . ?
H2A1 C2A H2A2 108.8 . . ?
C8A C7A C4A 114.3(19) . . ?
C8A C7A H7A1 108.7 . . ?
C4A C7A H7A1 108.7 . . ?
C8A C7A H7A2 108.7 . . ?
C4A C7A H7A2 108.7 . . ?
H7A1 C7A H7A2 107.6 . . ?
N1A C8A C7A 102.3(18) . . ?
N1A C8A H8A1 111.3 . . ?
C7A C8A H8A1 111.3 . . ?
N1A C8A H8A2 111.3 . . ?
C7A C8A H8A2 111.3 . . ?
H8A1 C8A H8A2 109.2 . . ?
C5A C4A C3A 107.9(9) . . ?
C5A C4A C7A 107.7(9) . . ?
C3A C4A C7A 107.4(9) . . ?
C5A C4A H4A 111.2 . . ?
C3A C4A H4A 111.2 . . ?
C7A C4A H4A 111.2 . . ?
C6A C5A C4A 108.6(18) . . ?
C6A C5A H5A1 110.0 . . ?
C4A C5A H5A1 110.0 . . ?
C6A C5A H5A2 110.0 . . ?
C4A C5A H5A2 110.0 . . ?
H5A1 C5A H5A2 108.4 . . ?
C2A C3A C4A 111.2(18) . . ?
C2A C3A H3A1 109.4 . . ?
C4A C3A H3A1 109.4 . . ?
C2A C3A H3A2 109.4 . . ?
C4A C3A H3A2 109.4 . . ?
H3A1 C3A H3A2 108.0 . . ?
N1A C6A C5A 108.6(18) . . ?
N1A C6A H6A1 110.0 . . ?
C5A C6A H6A1 110.0 . . ?
N1A C6A H6A2 110.0 . . ?
C5A C6A H6A2 110.0 . . ?
H6A1 C6A H6A2 108.4 . . ?
C2B N1B C6B 113.0(9) . . ?
C2B N1B C8B 112.7(9) . . ?
C6B N1B C8B 112.6(9) . . ?
C2B N1B H1B 106.3(12) . . ?
C6B N1B H1B 105.9(12) . . ?
C8B N1B H1B 105.6(12) . . ?
N1B C2B C3B 101.0(18) . . ?
N1B C2B H2B1 111.6 . . ?
C3B C2B H2B1 111.6 . . ?
N1B C2B H2B2 111.6 . . ?
C3B C2B H2B2 111.6 . . ?
H2B1 C2B H2B2 109.4 . . ?
C8B C7B C4B 108.1(15) . . ?
C8B C7B H7B1 110.1 . . ?
C4B C7B H7B1 110.1 . . ?
C8B C7B H7B2 110.1 . . ?
C4B C7B H7B2 110.1 . . ?
H7B1 C7B H7B2 108.4 . . ?
N1B C8B C7B 107.5(15) . . ?
N1B C8B H8B1 110.2 . . ?
C7B C8B H8B1 110.2 . . ?
N1B C8B H8B2 110.2 . . ?
C7B C8B H8B2 110.2 . . ?
H8B1 C8B H8B2 108.5 . . ?
C5B C4B C3B 108.0(9) . . ?
C5B C4B C7B 108.0(9) . . ?
C3B C4B C7B 107.7(9) . . ?
C5B C4B H4B 111.0 . . ?
C3B C4B H4B 111.0 . . ?
C7B C4B H4B 111.0 . . ?
C6B C5B C4B 108.5(16) . . ?
C6B C5B H5B1 110.0 . . ?
C4B C5B H5B1 110.0 . . ?
C6B C5B H5B2 110.0 . . ?
C4B C5B H5B2 110.0 . . ?
H5B1 C5B H5B2 108.4 . . ?
C2B C3B C4B 115.5(18) . . ?
C2B C3B H3B1 108.4 . . ?
C4B C3B H3B1 108.4 . . ?
C2B C3B H3B2 108.4 . . ?
C4B C3B H3B2 108.4 . . ?
H3B1 C3B H3B2 107.5 . . ?
N1B C6B C5B 108.0(16) . . ?
N1B C6B H6B1 110.1 . . ?
C5B C6B H6B1 110.1 . . ?
N1B C6B H6B2 110.1 . . ?
C5B C6B H6B2 110.1 . . ?
H6B1 C6B H6B2 108.4 . . ?

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
C8A N1A C2A C3A -68(2) . . . . ?
C6A N1A C2A C3A 62(2) . . . . ?
C6A N1A C8A C7A -63(2) . . . . ?
C2A N1A C8A C7A 67(2) . . . . ?
C4A C7A C8A N1A -1(2) . . . . ?
C8A C7A C4A C5A 59(2) . . . . ?
C8A C7A C4A C3A -57(2) . . . . ?
C3A C4A C5A C6A 60(2) . . . . ?
C7A C4A C5A C6A -56(2) . . . . ?
N1A C2A C3A C4A 2(2) . . . . ?
C5A C4A C3A C2A -61(2) . . . . ?
C7A C4A C3A C2A 55(2) . . . . ?
C8A N1A C6A C5A 67(2) . . . . ?
C2A N1A C6A C5A -63(2) . . . . ?
C4A C5A C6A N1A -1(2) . . . . ?
C6B N1B C2B C3B 69.6(19) . . . . ?
C8B N1B C2B C3B -59.4(19) . . . . ?
C2B N1B C8B C7B 74(2) . . . . ?
C6B N1B C8B C7B -55(2) . . . . ?
C4B C7B C8B N1B -11(2) . . . . ?
C8B C7B C4B C5B 68(2) . . . . ?
C8B C7B C4B C3B -49(2) . . . . ?
C3B C4B C5B C6B 59(2) . . . . ?
C7B C4B C5B C6B -57(2) . . . . ?
N1B C2B C3B C4B -9(2) . . . . ?
C5B C4B C3B C2B -52(2) . . . . ?
C7B C4B C3B C2B 64(2) . . . . ?
C2B N1B C6B C5B -63(2) . . . . ?
C8B N1B C6B C5B 66(2) . . . . ?
C4B C5B C6B N1B -7(3) . . . . ?

_refine_diff_density_max         1.958
_refine_diff_density_min         -1.384
_refine_diff_density_rms         0.330



####################################################################### 
# 
# 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_shelx_CCDC2
_database_code_depnum_ccdc_archive 'CCDC 2003978'
loop_
_audit_author_name
_audit_author_address
'Garikoitz Beobide'
;Universidad del Pais Vasco
Spain
;
_audit_update_record             
;
2020-05-14 deposited with the CCDC.	2020-06-12 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3

_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C7 H14 Cl4 Fe N'
_chemical_formula_weight         309.84

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Fe Fe 0.0000 0.0000
'Neutron Data Booklet, ILL Grenoble, France (2003) ISBN 0-9704143-7-4'
Cl Cl 0.0000 0.0000
'Neutron Data Booklet, ILL Grenoble, France (2003) ISBN 0-9704143-7-4'
N N 0.0000 0.0000
'Neutron Data Booklet, ILL Grenoble, France (2003) ISBN 0-9704143-7-4'
C C 0.0000 0.0000
'Neutron Data Booklet, ILL Grenoble, France (2003) ISBN 0-9704143-7-4'
H H 0.0000 0.0000
'Neutron Data Booklet, ILL Grenoble, France (2003) ISBN 0-9704143-7-4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'

_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+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'

_cell_length_a                   13.0822(5)
_cell_length_b                   12.5799(6)
_cell_length_c                   14.6292(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2407.57(17)
_cell_formula_units_Z            8
_cell_measurement_temperature    10(2)
_cell_measurement_reflns_used    3689
_cell_measurement_theta_min      5.43
_cell_measurement_theta_max      60.73

_exptl_crystal_description       Prism
_exptl_crystal_colour            Yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.710
_exptl_crystal_F_000             1256
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          2.200
_exptl_crystal_size_mid          2.100
_exptl_crystal_size_min          2.000
_exptl_absorpt_coefficient_mu    0.044
_shelx_estimated_absorpt_T_min   0.910
_shelx_estimated_absorpt_T_max   0.918
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      10(2)
_diffrn_radiation_wavelength     0.94558
_diffrn_radiation_type           neutrons
_diffrn_source                   ?
_diffrn_measurement_device_type  'D19, ILL'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            16006
_diffrn_reflns_av_unetI/netI     0.0269
_diffrn_reflns_av_R_equivalents  0.0438
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         4.673
_diffrn_reflns_theta_max         46.664
_diffrn_reflns_theta_full        34.566
_diffrn_measured_fraction_theta_max 0.856
_diffrn_measured_fraction_theta_full 0.905
_diffrn_reflns_Laue_measured_fraction_max 0.856
_diffrn_reflns_Laue_measured_fraction_full 0.905
_diffrn_reflns_point_group_measured_fraction_max 0.856
_diffrn_reflns_point_group_measured_fraction_full 0.905
_reflns_number_total             3921
_reflns_number_gt                3821
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+188.9306P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_extinction_coef       ?
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         3921
_refine_ls_number_parameters     245
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0975
_refine_ls_R_factor_gt           0.0961
_refine_ls_wR_factor_ref         0.2262
_refine_ls_wR_factor_gt          0.2256
_refine_ls_goodness_of_fit_ref   1.254
_refine_ls_restrained_S_all      1.254
_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 0.28330(12) 0.04255(14) 0.24909(10) 0.0057(3) Uani 1 1 d . . . . .
Cl4 Cl 0.20122(12) -0.01100(16) 0.37105(10) 0.0097(3) Uani 1 1 d . . . . .
Cl2 Cl 0.44191(12) -0.01459(15) 0.25615(10) 0.0082(3) Uani 1 1 d . . . . .
Cl1 Cl 0.21655(12) -0.02161(14) 0.12186(10) 0.0081(3) Uani 1 1 d . . . . .
Cl3 Cl 0.27885(14) 0.21760(15) 0.24210(11) 0.0104(3) Uani 1 1 d . . . . .
N1 N 0.09744(13) 0.29621(16) 0.08231(11) 0.0086(3) Uani 1 1 d . . . . .
C7 C -0.0185(2) 0.3359(2) -0.04673(16) 0.0113(4) Uani 1 1 d . . . . .
C3 C 0.0984(2) 0.1802(2) -0.05438(17) 0.0117(5) Uani 1 1 d . . . . .
C2 C 0.16518(18) 0.2450(2) 0.01175(16) 0.0099(4) Uani 1 1 d . . . . .
C6 C 0.02804(19) 0.2149(2) 0.12516(15) 0.0117(5) Uani 1 1 d . . . . .
C4 C -0.01346(19) 0.2143(2) -0.04198(15) 0.0103(4) Uani 1 1 d . . . . .
C5 C -0.0496(2) 0.1782(3) 0.05261(16) 0.0143(5) Uani 1 1 d . . . . .
C8 C 0.03510(18) 0.3824(2) 0.03761(15) 0.0092(4) Uani 1 1 d . . . . .
H71 H -0.0982(5) 0.3620(7) -0.0488(5) 0.0290(13) Uani 1 1 d . . . . .
H72 H 0.0179(6) 0.3651(6) -0.1095(4) 0.0264(12) Uani 1 1 d . . . . .
H31 H 0.1246(6) 0.1938(7) -0.1235(4) 0.0295(14) Uani 1 1 d . . . . .
H32 H 0.1070(6) 0.0950(6) -0.0403(5) 0.0318(14) Uani 1 1 d . . . . .
H21 H 0.2202(5) 0.1953(7) 0.0487(4) 0.0275(13) Uani 1 1 d . . . . .
H22 H 0.2063(5) 0.3087(6) -0.0229(4) 0.0244(11) Uani 1 1 d . . . . .
H61 H -0.0073(5) 0.2522(7) 0.1852(4) 0.0274(13) Uani 1 1 d . . . . .
H62 H 0.0761(5) 0.1501(6) 0.1488(4) 0.0257(12) Uani 1 1 d . . . . .
H4 H -0.0598(5) 0.1788(6) -0.0952(4) 0.0255(12) Uani 1 1 d . . . . .
H51 H -0.1254(5) 0.2111(8) 0.0676(5) 0.0337(17) Uani 1 1 d . . . . .
H52 H -0.0592(7) 0.0912(7) 0.0557(5) 0.0361(17) Uani 1 1 d . . . . .
H81 H 0.0880(5) 0.4463(6) 0.0208(5) 0.0263(12) Uani 1 1 d . . . . .
H82 H -0.0175(5) 0.4106(6) 0.0896(4) 0.0259(12) Uani 1 1 d . . . . .
H1 H 0.1422(4) 0.3296(5) 0.1320(4) 0.0199(10) Uani 1 1 d . . . . .


_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 Cl4 2.189(2) . ?
Fe1 Cl2 2.198(2) . ?
Fe1 Cl3 2.205(3) . ?
Fe1 Cl1 2.209(2) . ?
N1 H1 1.024(6) . ?
N1 C6 1.505(3) . ?
N1 C2 1.505(3) . ?
N1 C8 1.506(3) . ?
C7 H71 1.093(7) . ?
C7 H72 1.098(7) . ?
C7 C4 1.532(4) . ?
C7 C8 1.535(3) . ?
C3 H31 1.081(7) . ?
C3 H32 1.097(8) . ?
C3 C4 1.536(4) . ?
C3 C2 1.538(4) . ?
C2 H22 1.091(7) . ?
C2 H21 1.096(7) . ?
C6 H62 1.086(7) . ?
C6 H61 1.098(7) . ?
C6 C5 1.540(4) . ?
C4 H4 1.083(6) . ?
C4 C5 1.531(3) . ?
C5 H51 1.097(8) . ?
C5 H52 1.102(9) . ?
C8 H82 1.086(6) . ?
C8 H81 1.089(7) . ?

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
Cl4 Fe1 Cl2 108.91(9) . . ?
Cl4 Fe1 Cl3 109.40(10) . . ?
Cl2 Fe1 Cl3 110.71(10) . . ?
Cl4 Fe1 Cl1 112.36(9) . . ?
Cl2 Fe1 Cl1 107.05(9) . . ?
Cl3 Fe1 Cl1 108.38(9) . . ?
H1 N1 C6 109.1(4) . . ?
H1 N1 C2 109.0(4) . . ?
C6 N1 C2 110.5(2) . . ?
H1 N1 C8 108.9(4) . . ?
C6 N1 C8 110.08(17) . . ?
C2 N1 C8 109.22(16) . . ?
H71 C7 H72 106.8(6) . . ?
H71 C7 C4 110.0(5) . . ?
H72 C7 C4 110.7(4) . . ?
H71 C7 C8 110.1(4) . . ?
H72 C7 C8 110.3(4) . . ?
C4 C7 C8 108.9(2) . . ?
H31 C3 H32 107.4(7) . . ?
H31 C3 C4 111.6(5) . . ?
H32 C3 C4 110.4(5) . . ?
H31 C3 C2 109.0(5) . . ?
H32 C3 C2 110.0(4) . . ?
C4 C3 C2 108.6(2) . . ?
H22 C2 H21 108.9(6) . . ?
H22 C2 N1 107.2(4) . . ?
H21 C2 N1 107.0(4) . . ?
H22 C2 C3 112.2(4) . . ?
H21 C2 C3 112.3(5) . . ?
N1 C2 C3 108.91(18) . . ?
H62 C6 H61 108.1(6) . . ?
H62 C6 N1 107.0(4) . . ?
H61 C6 N1 107.3(5) . . ?
H62 C6 C5 112.1(5) . . ?
H61 C6 C5 113.7(4) . . ?
N1 C6 C5 108.34(18) . . ?
H4 C4 C5 110.7(4) . . ?
H4 C4 C7 110.8(4) . . ?
C5 C4 C7 108.9(2) . . ?
H4 C4 C3 109.5(4) . . ?
C5 C4 C3 108.5(2) . . ?
C7 C4 C3 108.4(2) . . ?
H51 C5 H52 105.3(8) . . ?
H51 C5 C4 110.3(5) . . ?
H52 C5 C4 111.5(5) . . ?
H51 C5 C6 110.2(5) . . ?
H52 C5 C6 110.1(5) . . ?
C4 C5 C6 109.3(2) . . ?
H82 C8 H81 108.6(6) . . ?
H82 C8 N1 106.0(4) . . ?
H81 C8 N1 106.6(4) . . ?
H82 C8 C7 113.4(4) . . ?
H81 C8 C7 113.0(4) . . ?
N1 C8 C7 108.8(2) . . ?

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
H1 N1 C2 H22 -67.2(6) . . . . ?
C6 N1 C2 H22 172.8(4) . . . . ?
C8 N1 C2 H22 51.6(4) . . . . ?
H1 N1 C2 H21 49.5(7) . . . . ?
C6 N1 C2 H21 -70.4(5) . . . . ?
C8 N1 C2 H21 168.3(5) . . . . ?
H1 N1 C2 C3 171.2(4) . . . . ?
C6 N1 C2 C3 51.2(2) . . . . ?
C8 N1 C2 C3 -70.0(2) . . . . ?
H31 C3 C2 H22 18.6(7) . . . . ?
H32 C3 C2 H22 136.0(7) . . . . ?
C4 C3 C2 H22 -103.1(5) . . . . ?
H31 C3 C2 H21 -104.6(7) . . . . ?
H32 C3 C2 H21 12.8(7) . . . . ?
C4 C3 C2 H21 133.7(4) . . . . ?
H31 C3 C2 N1 137.0(5) . . . . ?
H32 C3 C2 N1 -105.6(5) . . . . ?
C4 C3 C2 N1 15.3(3) . . . . ?
H1 N1 C6 H62 -67.5(6) . . . . ?
C2 N1 C6 H62 52.4(5) . . . . ?
C8 N1 C6 H62 173.1(4) . . . . ?
H1 N1 C6 H61 48.3(6) . . . . ?
C2 N1 C6 H61 168.2(4) . . . . ?
C8 N1 C6 H61 -71.1(5) . . . . ?
H1 N1 C6 C5 171.4(4) . . . . ?
C2 N1 C6 C5 -68.7(3) . . . . ?
C8 N1 C6 C5 52.0(3) . . . . ?
H71 C7 C4 H4 51.1(6) . . . . ?
H72 C7 C4 H4 -66.7(6) . . . . ?
C8 C7 C4 H4 171.9(4) . . . . ?
H71 C7 C4 C5 -70.9(5) . . . . ?
H72 C7 C4 C5 171.3(4) . . . . ?
C8 C7 C4 C5 49.8(3) . . . . ?
H71 C7 C4 C3 171.2(4) . . . . ?
H72 C7 C4 C3 53.4(5) . . . . ?
C8 C7 C4 C3 -68.0(2) . . . . ?
H31 C3 C4 H4 51.0(7) . . . . ?
H32 C3 C4 H4 -68.3(6) . . . . ?
C2 C3 C4 H4 171.0(4) . . . . ?
H31 C3 C4 C5 171.9(5) . . . . ?
H32 C3 C4 C5 52.6(5) . . . . ?
C2 C3 C4 C5 -68.0(3) . . . . ?
H31 C3 C4 C7 -69.9(6) . . . . ?
H32 C3 C4 C7 170.8(5) . . . . ?
C2 C3 C4 C7 50.1(3) . . . . ?
H4 C4 C5 H51 -67.9(8) . . . . ?
C7 C4 C5 H51 54.2(6) . . . . ?
C3 C4 C5 H51 171.9(6) . . . . ?
H4 C4 C5 H52 48.8(7) . . . . ?
C7 C4 C5 H52 170.8(6) . . . . ?
C3 C4 C5 H52 -71.4(6) . . . . ?
H4 C4 C5 C6 170.8(5) . . . . ?
C7 C4 C5 C6 -67.2(3) . . . . ?
C3 C4 C5 C6 50.6(3) . . . . ?
H62 C6 C5 H51 134.9(7) . . . . ?
H61 C6 C5 H51 11.9(8) . . . . ?
N1 C6 C5 H51 -107.2(6) . . . . ?
H62 C6 C5 H52 19.1(7) . . . . ?
H61 C6 C5 H52 -103.8(8) . . . . ?
N1 C6 C5 H52 137.0(6) . . . . ?
H62 C6 C5 C4 -103.7(5) . . . . ?
H61 C6 C5 C4 133.3(5) . . . . ?
N1 C6 C5 C4 14.2(3) . . . . ?
H1 N1 C8 H82 -66.8(6) . . . . ?
C6 N1 C8 H82 52.8(5) . . . . ?
C2 N1 C8 H82 174.2(4) . . . . ?
H1 N1 C8 H81 48.8(6) . . . . ?
C6 N1 C8 H81 168.3(4) . . . . ?
C2 N1 C8 H81 -70.2(5) . . . . ?
H1 N1 C8 C7 170.8(4) . . . . ?
C6 N1 C8 C7 -69.6(2) . . . . ?
C2 N1 C8 C7 51.9(2) . . . . ?
H71 C7 C8 H82 17.8(7) . . . . ?
H72 C7 C8 H82 135.5(7) . . . . ?
C4 C7 C8 H82 -102.9(5) . . . . ?
H71 C7 C8 H81 -106.4(7) . . . . ?
H72 C7 C8 H81 11.2(7) . . . . ?
C4 C7 C8 H81 132.9(5) . . . . ?
H71 C7 C8 N1 135.5(5) . . . . ?
H72 C7 C8 N1 -106.9(5) . . . . ?
C4 C7 C8 N1 14.8(3) . . . . ?

_refine_diff_density_max         3.298
_refine_diff_density_min         -2.240
_refine_diff_density_rms         0.430



####################################################################### 
# 
# 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_shelx_CCDC3
_database_code_depnum_ccdc_archive 'CCDC 2003980'
loop_
_audit_author_name
_audit_author_address
'Garikoitz Beobide'
;Universidad del Pais Vasco
Spain
;
_audit_update_record             
;
2020-05-14 deposited with the CCDC.	2020-06-12 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7

_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C7 H14 Cl4 Fe1 N1'
_chemical_formula_weight         309.84

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      orthorhombic
_space_group_IT_number           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'

_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+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z'
'x, -y-1/2, z-1/2'

_cell_length_a                   13.1204(3)
_cell_length_b                   12.6450(4)
_cell_length_c                   14.7155(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2441.41(13)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    3507
_cell_measurement_theta_min      3.3690
_cell_measurement_theta_max      25.0270

_exptl_crystal_description       Prism
_exptl_crystal_colour            Yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.686
_exptl_crystal_F_000             1256
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.11
_exptl_absorpt_coefficient_mu    2.068
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_T_min  0.374
_exptl_absorpt_correction_T_max  0.780
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.558
_oxdiff_exptl_absorpt_empirical_full_max 1.418
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            19585
_diffrn_reflns_av_unetI/netI     0.0403
_diffrn_reflns_av_R_equivalents  0.0694
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.631
_diffrn_reflns_theta_max         27.317
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.945
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.945
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.945
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             2606
_reflns_number_gt                2246
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0099P)²+20.9373P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2606
_refine_ls_number_parameters     121
_refine_ls_number_restraints     36
_refine_ls_R_factor_all          0.0731
_refine_ls_R_factor_gt           0.0640
_refine_ls_wR_factor_ref         0.1244
_refine_ls_wR_factor_gt          0.1203
_refine_ls_goodness_of_fit_ref   1.178
_refine_ls_restrained_S_all      1.184
_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 0.28199(6) 0.04151(6) 0.24894(5) 0.01395(19) Uani 1 1 d . . . . .
Cl14 Cl 0.20105(10) -0.01204(12) 0.37014(9) 0.0267(3) Uani 1 1 d . . . . .
Cl12 Cl 0.44040(9) -0.01403(11) 0.25590(8) 0.0195(3) Uani 1 1 d . . . . .
Cl11 Cl 0.21535(10) -0.02272(10) 0.12302(8) 0.0194(3) Uani 1 1 d . . . . .
Cl13 Cl 0.27688(12) 0.21531(10) 0.24226(10) 0.0285(3) Uani 1 1 d . . . . .
N11 N 0.0963(4) 0.2966(4) 0.0817(3) 0.0210(9) Uani 1 1 d . U . . .
C17 C -0.0218(5) 0.3351(5) -0.0439(5) 0.0362(16) Uani 1 1 d . . . . .
H17A H -0.0928 0.3563 -0.0413 0.043 Uiso 1 1 calc R U . . .
H17B H 0.0069 0.3610 -0.1004 0.043 Uiso 1 1 calc R U . . .
C13 C 0.0967(5) 0.1845(5) -0.0553(4) 0.0317(12) Uani 1 1 d . U . . .
H13A H 0.1173 0.2015 -0.1169 0.038 Uiso 1 1 calc R U . . .
H13B H 0.1047 0.1089 -0.0465 0.038 Uiso 1 1 calc R U . . .
C12 C 0.1638(4) 0.2445(5) 0.0125(4) 0.0225(10) Uani 1 1 d . U . . .
H12A H 0.2102 0.1959 0.0424 0.027 Uiso 1 1 calc R U . . .
H12B H 0.2039 0.2975 -0.0190 0.027 Uiso 1 1 calc R U . . .
C16 C 0.0252(4) 0.2173(5) 0.1247(4) 0.0249(11) Uani 1 1 d . U . . .
H16A H -0.0130 0.2507 0.1733 0.030 Uiso 1 1 calc R U . . .
H16B H 0.0641 0.1593 0.1504 0.030 Uiso 1 1 calc R U . . .
C14 C -0.0143(5) 0.2158(5) -0.0408(4) 0.0273(11) Uani 1 1 d . U . . .
H14 H -0.0572 0.1846 -0.0882 0.033 Uiso 1 1 calc R U . . .
C15 C -0.0475(5) 0.1758(6) 0.0526(4) 0.0391(15) Uani 1 1 d . U . . .
H15A H -0.1162 0.1998 0.0655 0.047 Uiso 1 1 calc R U . . .
H15B H -0.0474 0.0991 0.0531 0.047 Uiso 1 1 calc R U . . .
C18 C 0.0364(4) 0.3826(4) 0.0370(4) 0.0226(12) Uani 1 1 d . . . . .
H18A H 0.0818 0.4380 0.0160 0.027 Uiso 1 1 calc R U . . .
H18B H -0.0112 0.4133 0.0800 0.027 Uiso 1 1 calc R U . . .
H11 H 0.144(5) 0.327(5) 0.120(4) 0.027 Uiso 1 1 d . 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 Cl14 2.1833(15) . ?
Fe1 Cl12 2.1963(14) . ?
Fe1 Cl13 2.2008(15) . ?
Fe1 Cl11 2.2040(14) . ?
N11 C18 1.495(7) . ?
N11 C12 1.501(7) . ?
N11 C16 1.509(7) . ?
N11 H11 0.93(6) . ?
C17 C14 1.512(9) . ?
C17 C18 1.536(8) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C13 C14 1.525(9) . ?
C13 C12 1.532(8) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C16 C15 1.521(8) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C14 C15 1.528(8) . ?
C14 H14 0.9800 . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C18 H18A 0.9700 . ?
C18 H18B 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_3
_geom_angle_publ_flag
Cl14 Fe1 Cl12 108.85(6) . . ?
Cl14 Fe1 Cl13 109.35(7) . . ?
Cl12 Fe1 Cl13 110.50(6) . . ?
Cl14 Fe1 Cl11 112.30(6) . . ?
Cl12 Fe1 Cl11 107.26(6) . . ?
Cl13 Fe1 Cl11 108.56(6) . . ?
C18 N11 C12 109.4(4) . . ?
C18 N11 C16 110.1(4) . . ?
C12 N11 C16 111.0(4) . . ?
C18 N11 H11 109(4) . . ?
C12 N11 H11 102(4) . . ?
C16 N11 H11 116(4) . . ?
C14 C17 C18 109.6(5) . . ?
C14 C17 H17A 109.8 . . ?
C18 C17 H17A 109.8 . . ?
C14 C17 H17B 109.8 . . ?
C18 C17 H17B 109.8 . . ?
H17A C17 H17B 108.2 . . ?
C14 C13 C12 109.2(5) . . ?
C14 C13 H13A 109.8 . . ?
C12 C13 H13A 109.8 . . ?
C14 C13 H13B 109.8 . . ?
C12 C13 H13B 109.8 . . ?
H13A C13 H13B 108.3 . . ?
N11 C12 C13 108.7(4) . . ?
N11 C12 H12A 110.0 . . ?
C13 C12 H12A 110.0 . . ?
N11 C12 H12B 110.0 . . ?
C13 C12 H12B 110.0 . . ?
H12A C12 H12B 108.3 . . ?
N11 C16 C15 108.9(5) . . ?
N11 C16 H16A 109.9 . . ?
C15 C16 H16A 109.9 . . ?
N11 C16 H16B 109.9 . . ?
C15 C16 H16B 109.9 . . ?
H16A C16 H16B 108.3 . . ?
C17 C14 C13 108.5(5) . . ?
C17 C14 C15 109.8(6) . . ?
C13 C14 C15 108.2(5) . . ?
C17 C14 H14 110.1 . . ?
C13 C14 H14 110.1 . . ?
C15 C14 H14 110.1 . . ?
C16 C15 C14 109.6(5) . . ?
C16 C15 H15A 109.8 . . ?
C14 C15 H15A 109.8 . . ?
C16 C15 H15B 109.8 . . ?
C14 C15 H15B 109.8 . . ?
H15A C15 H15B 108.2 . . ?
N11 C18 C17 108.5(5) . . ?
N11 C18 H18A 110.0 . . ?
C17 C18 H18A 110.0 . . ?
N11 C18 H18B 110.0 . . ?
C17 C18 H18B 110.0 . . ?
H18A C18 H18B 108.4 . . ?

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
C18 N11 C12 C13 -68.0(6) . . . . ?
C16 N11 C12 C13 53.6(6) . . . . ?
C14 C13 C12 N11 11.1(7) . . . . ?
C18 N11 C16 C15 56.0(6) . . . . ?
C12 N11 C16 C15 -65.2(6) . . . . ?
C18 C17 C14 C13 -65.5(7) . . . . ?
C18 C17 C14 C15 52.6(7) . . . . ?
C12 C13 C14 C17 52.8(7) . . . . ?
C12 C13 C14 C15 -66.3(6) . . . . ?
N11 C16 C15 C14 8.1(8) . . . . ?
C17 C14 C15 C16 -63.5(7) . . . . ?
C13 C14 C15 C16 54.8(7) . . . . ?
C12 N11 C18 C17 55.4(6) . . . . ?
C16 N11 C18 C17 -66.8(6) . . . . ?
C14 C17 C18 N11 10.1(7) . . . . ?

_refine_diff_density_max         0.782
_refine_diff_density_min         -0.620
_refine_diff_density_rms         0.131



