# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# 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_ZnCl4
_database_code_depnum_ccdc_archive 'CCDC 1585681'
_audit_update_record             
;
2017-11-14 deposited with the CCDC.
2018-05-11 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT360_ZnCl4               
;
PROBLEM: Short  C(sp3)-C(sp3) Bond  C7       - C8       .       1.22 Ang.
RESPONSE: Deviating bond distance due to unresolved disorder typical for this molecule. Structure identity is confirmed through isostructurality with published structures.
;
_vrf_PLAT241_ZnCl4               
;
PROBLEM: High   'MainMol' Ueq as Compared to Neighbors of         C7 Check
RESPONSE: Deviating bond distance due to unresolved disorder typical for this molecule. Structure identity is confirmed through isostructurality with published structures.
;
_vrf_PLAT242_ZnCl4               
;
PROBLEM: Low    'MainMol' Ueq as Compared to Neighbors of         N2 Check
RESPONSE: Deviating bond distance due to unresolved disorder typical for this molecule. Structure identity is confirmed through isostructurality with published structures.
;
# Added during the CSD deposition process: Tuesday 14 November 2017 08:41 PM
# end Validation Reply Form


_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        'Triethylammonium tetrachlorozincate'
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C3 H16 N +), Zn Cl4 -'
_chemical_formula_sum            'C12 H32 Cl4 N2 Zn'
_chemical_formula_weight         411.56

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'
Zn Zn 0.2839 1.4301 '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                   12.0090(11)
_cell_length_b                   13.2871(13)
_cell_length_c                   25.952(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4141.0(7)
_cell_formula_units_Z            8
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    8015
_cell_measurement_theta_min      2.31
_cell_measurement_theta_max      19.51

_exptl_crystal_description       needle
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.320
_exptl_crystal_F_000             1728
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.03
_exptl_absorpt_coefficient_mu    1.694
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3644
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_process_details   'Bruker AXScale'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            84236
_diffrn_reflns_av_unetI/netI     0.0621
_diffrn_reflns_av_R_equivalents  0.1710
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_theta_min         1.569
_diffrn_reflns_theta_max         26.524
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             4260
_reflns_number_gt                2413
_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       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
'Room temperature data set with unresolved disorder'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0899P)²+6.1531P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4260
_refine_ls_number_parameters     184
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1338
_refine_ls_R_factor_gt           0.0698
_refine_ls_wR_factor_ref         0.1973
_refine_ls_wR_factor_gt          0.1597
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_restrained_S_all      1.015
_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
Zn1 Zn 0.05295(6) 0.28337(5) 0.12634(2) 0.0584(3) Uani 1 1 d . . . . .
Cl1 Cl 0.21917(14) 0.32180(16) 0.09073(7) 0.0855(6) Uani 1 1 d . . . . .
Cl2 Cl -0.06816(15) 0.41180(13) 0.12351(7) 0.0825(5) Uani 1 1 d . . . . .
Cl3 Cl 0.08149(15) 0.24038(17) 0.21063(7) 0.0914(6) Uani 1 1 d . . . . .
Cl4 Cl -0.02101(18) 0.15224(15) 0.08090(8) 0.1037(8) Uani 1 1 d . . . . .
N1 N 0.3825(4) 0.6905(4) -0.0231(2) 0.0667(14) Uani 1 1 d . . . . .
H1 H 0.416(5) 0.687(5) 0.009(3) 0.080 Uiso 1 1 d . U . . .
N2 N 0.2543(4) 0.0611(4) 0.2357(2) 0.0697(14) Uani 1 1 d . . . . .
H2 H 0.210(6) 0.108(5) 0.224(3) 0.084 Uiso 1 1 d . U . . .
C1 C 0.4617(6) 0.6292(5) -0.0548(3) 0.091(2) Uani 1 1 d . . . . .
H1A H 0.4666 0.5621 -0.0403 0.109 Uiso 1 1 calc R U . . .
H1B H 0.5352 0.6594 -0.0528 0.109 Uiso 1 1 calc R U . . .
C2 C 0.4280(10) 0.6212(8) -0.1106(4) 0.146(4) Uani 1 1 d . . . . .
H2A H 0.3572 0.5880 -0.1130 0.220 Uiso 1 1 calc R U . . .
H2B H 0.4829 0.5831 -0.1291 0.220 Uiso 1 1 calc R U . . .
H2C H 0.4225 0.6874 -0.1252 0.220 Uiso 1 1 calc R U . . .
C3 C 0.3741(7) 0.7996(5) -0.0396(3) 0.085(2) Uani 1 1 d . . . . .
H3A H 0.3528 0.8024 -0.0757 0.102 Uiso 1 1 calc R U . . .
H3B H 0.3161 0.8325 -0.0198 0.102 Uiso 1 1 calc R U . . .
C4 C 0.4816(7) 0.8558(6) -0.0325(3) 0.102(3) Uani 1 1 d . . . . .
H4A H 0.5018 0.8553 0.0033 0.153 Uiso 1 1 calc R U . . .
H4B H 0.4725 0.9241 -0.0438 0.153 Uiso 1 1 calc R U . . .
H4C H 0.5392 0.8240 -0.0523 0.153 Uiso 1 1 calc R U . . .
C5 C 0.2682(6) 0.6460(6) -0.0189(3) 0.093(2) Uani 1 1 d . . . . .
H5A H 0.2219 0.6898 0.0020 0.112 Uiso 1 1 calc R U . . .
H5B H 0.2353 0.6421 -0.0530 0.112 Uiso 1 1 calc R U . . .
C6 C 0.2700(7) 0.5434(6) 0.0046(4) 0.128(3) Uani 1 1 d . . . . .
H6A H 0.3139 0.4993 -0.0165 0.192 Uiso 1 1 calc R U . . .
H6B H 0.1953 0.5180 0.0069 0.192 Uiso 1 1 calc R U . . .
H6C H 0.3020 0.5471 0.0384 0.192 Uiso 1 1 calc R U . . .
C7 C 0.1805(13) -0.0266(9) 0.2476(5) 0.209(8) Uani 1 1 d . . . . .
H7A H 0.2275 -0.0740 0.2659 0.250 Uiso 1 1 calc R U . . .
H7B H 0.1275 -0.0016 0.2727 0.250 Uiso 1 1 calc R U . . .
C8 C 0.1256(12) -0.0779(12) 0.2179(6) 0.223(9) Uani 1 1 d . . . . .
H8A H 0.0489 -0.0770 0.2283 0.334 Uiso 1 1 calc R U . . .
H8B H 0.1527 -0.1458 0.2184 0.334 Uiso 1 1 calc R U . . .
H8C H 0.1321 -0.0511 0.1836 0.334 Uiso 1 1 calc R U . . .
C9 C 0.3326(7) 0.0399(7) 0.1923(3) 0.105(3) Uani 1 1 d . . . . .
H9A H 0.3885 -0.0075 0.2042 0.126 Uiso 1 1 calc R U . . .
H9B H 0.2914 0.0077 0.1647 0.126 Uiso 1 1 calc R U . . .
C10 C 0.3891(7) 0.1289(6) 0.1715(3) 0.113(3) Uani 1 1 d . . . . .
H10A H 0.3349 0.1791 0.1628 0.170 Uiso 1 1 calc R U . . .
H10B H 0.4303 0.1104 0.1412 0.170 Uiso 1 1 calc R U . . .
H10C H 0.4393 0.1554 0.1969 0.170 Uiso 1 1 calc R U . . .
C11 C 0.3135(7) 0.0935(8) 0.2827(3) 0.110(3) Uani 1 1 d . . . . .
H11A H 0.3490 0.0350 0.2980 0.132 Uiso 1 1 calc R U . . .
H11B H 0.3721 0.1399 0.2728 0.132 Uiso 1 1 calc R U . . .
C12 C 0.2444(7) 0.1421(7) 0.3222(3) 0.109(3) Uani 1 1 d . . . . .
H12A H 0.2088 0.2003 0.3078 0.163 Uiso 1 1 calc R U . . .
H12B H 0.2904 0.1622 0.3507 0.163 Uiso 1 1 calc R U . . .
H12C H 0.1888 0.0957 0.3341 0.163 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
Zn1 Cl2 2.2433(17) . ?
Zn1 Cl1 2.2583(18) . ?
Zn1 Cl4 2.2837(19) . ?
Zn1 Cl3 2.2866(19) . ?
N1 C5 1.498(9) . ?
N1 C1 1.499(8) . ?
N1 C3 1.516(8) . ?
N2 C11 1.476(9) . ?
N2 C9 1.494(8) . ?
N2 C7 1.496(11) . ?
C1 C2 1.507(12) . ?
C3 C4 1.503(10) . ?
C5 C6 1.493(11) . ?
C7 C8 1.222(15) . ?
C9 C10 1.467(11) . ?
C11 C12 1.470(10) . ?

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
Cl2 Zn1 Cl1 112.81(8) . . ?
Cl2 Zn1 Cl4 108.14(8) . . ?
Cl1 Zn1 Cl4 107.75(7) . . ?
Cl2 Zn1 Cl3 108.58(7) . . ?
Cl1 Zn1 Cl3 108.39(7) . . ?
Cl4 Zn1 Cl3 111.20(9) . . ?
C5 N1 C1 114.0(5) . . ?
C5 N1 C3 109.7(5) . . ?
C1 N1 C3 113.9(6) . . ?
C11 N2 C9 112.0(6) . . ?
C11 N2 C7 110.1(8) . . ?
C9 N2 C7 112.4(6) . . ?
N1 C1 C2 113.3(6) . . ?
C4 C3 N1 112.5(6) . . ?
C6 C5 N1 112.1(6) . . ?
C8 C7 N2 128.7(14) . . ?
C10 C9 N2 114.6(7) . . ?
C12 C11 N2 115.6(6) . . ?

_refine_diff_density_max         0.917
_refine_diff_density_min         -0.662
_refine_diff_density_rms         0.085

_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Ethanol'
####################################################################### 
# 
# 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_AlCl4
_database_code_depnum_ccdc_archive 'CCDC 1585682'
_audit_update_record             
;
2017-11-14 deposited with the CCDC.
2018-05-11 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT242_AlCl4               
;
PROBLEM: Low    'MainMol' Ueq as Compared to Neighbors of         Al Check
RESPONSE: This can be due to greater thermal motion of the terminal chlorides vs. restricted motion of the had, centrally-bound Al cation.
;
_vrf_PLAT790_AlCl4               
;
PROBLEM: Centre of Gravity not Within Unit Cell: Resd.  #          1 Note
RESPONSE: Residue 1 positioned to illustrate major hydrogen bond.
;
# Added during the CSD deposition process: Tuesday 14 November 2017 08:41 PM
# end Validation Reply Form


_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        'Triethylammonium tetrachloroaluminate'
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C6 H16 N +, Al Cl4 -'
_chemical_formula_sum            'C6 H16 Al Cl4 N'
_chemical_formula_weight         270.98

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'
Al Al 0.0645 0.0514 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

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

_cell_length_a                   7.607(2)
_cell_length_b                   12.693(4)
_cell_length_c                   14.162(3)
_cell_angle_alpha                90
_cell_angle_beta                 97.859(17)
_cell_angle_gamma                90
_cell_volume                     1354.6(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    3445
_cell_measurement_theta_min      2.89
_cell_measurement_theta_max      23.03

_exptl_crystal_description       needle
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.329
_exptl_crystal_F_000             560
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.010
_exptl_absorpt_coefficient_mu    0.898
_shelx_estimated_absorpt_T_min   0.855
_shelx_estimated_absorpt_T_max   0.991
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6896
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   'Bruker AXScale'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            14143
_diffrn_reflns_av_unetI/netI     0.0700
_diffrn_reflns_av_R_equivalents  0.0566
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.164
_diffrn_reflns_theta_max         27.558
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measured_fraction_theta_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_point_group_measured_fraction_full 0.993
_reflns_number_total             3103
_reflns_number_gt                1841
_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       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_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)+(0.0394P)²+0.0213P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3103
_refine_ls_number_parameters     115
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1004
_refine_ls_R_factor_gt           0.0437
_refine_ls_wR_factor_ref         0.0989
_refine_ls_wR_factor_gt          0.0825
_refine_ls_goodness_of_fit_ref   0.991
_refine_ls_restrained_S_all      0.991
_refine_ls_shift/su_max          0.001
_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
Cl1 Cl 0.19575(10) 0.81519(5) 0.71731(5) 0.0468(2) Uani 1 1 d . . . . .
Cl2 Cl -0.05154(11) 1.03394(6) 0.63864(5) 0.0509(2) Uani 1 1 d . . . . .
Cl3 Cl 0.16745(12) 1.02410(6) 0.87219(4) 0.0560(3) Uani 1 1 d . . . . .
Cl4 Cl 0.41032(11) 1.05027(6) 0.68230(5) 0.0494(2) Uani 1 1 d . . . . .
Al Al 0.18114(12) 0.98320(6) 0.72821(5) 0.0346(2) Uani 1 1 d . . . . .
N1 N -0.2192(3) 0.76202(19) 0.61674(13) 0.0369(6) Uani 1 1 d . . . . .
H1C H -0.120(4) 0.798(2) 0.6366(18) 0.055 Uiso 1 1 d . U . . .
C1 C -0.1521(4) 0.6690(2) 0.56760(18) 0.0482(8) Uani 1 1 d . . . . .
H1A H -0.2529 0.6219 0.5452 0.058 Uiso 1 1 calc R U . . .
H1B H -0.0678 0.6292 0.6137 0.058 Uiso 1 1 calc R U . . .
C2 C -0.0612(5) 0.7004(3) 0.48417(18) 0.0637(10) Uani 1 1 d . . . . .
H2A H -0.0054 0.6383 0.4597 0.096 Uiso 1 1 calc R U . . .
H2B H 0.0298 0.7534 0.5045 0.096 Uiso 1 1 calc R U . . .
H2C H -0.1486 0.7298 0.4338 0.096 Uiso 1 1 calc R U . . .
C3 C -0.3470(4) 0.8315(2) 0.55391(17) 0.0458(8) Uani 1 1 d . . . . .
H3A H -0.2843 0.8634 0.5042 0.055 Uiso 1 1 calc R U . . .
H3B H -0.3862 0.8894 0.5929 0.055 Uiso 1 1 calc R U . . .
C4 C -0.5088(4) 0.7732(3) 0.5062(2) 0.0607(10) Uani 1 1 d . . . . .
H4A H -0.5919 0.8235 0.4717 0.091 Uiso 1 1 calc R U . . .
H4B H -0.5668 0.7369 0.5546 0.091 Uiso 1 1 calc R U . . .
H4C H -0.4725 0.7215 0.4612 0.091 Uiso 1 1 calc R U . . .
C5 C -0.2881(4) 0.7259(2) 0.70609(16) 0.0446(8) Uani 1 1 d . . . . .
H5A H -0.4086 0.6962 0.6890 0.054 Uiso 1 1 calc R U . . .
H5B H -0.2104 0.6692 0.7362 0.054 Uiso 1 1 calc R U . . .
C6 C -0.2953(4) 0.8131(3) 0.77613(18) 0.0538(9) Uani 1 1 d . . . . .
H6A H -0.3311 0.7848 0.8350 0.081 Uiso 1 1 calc R U . . .
H6B H -0.3817 0.8660 0.7492 0.081 Uiso 1 1 calc R U . . .
H6C H -0.1779 0.8458 0.7902 0.081 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
Cl1 Al 2.1421(12) . ?
Cl2 Al 2.1314(12) . ?
Cl3 Al 2.1204(11) . ?
Cl4 Al 2.1206(13) . ?
N1 C1 1.495(3) . ?
N1 C5 1.506(3) . ?
N1 C3 1.510(3) . ?
C1 C2 1.502(3) . ?
C3 C4 1.514(4) . ?
C5 C6 1.492(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cl3 Al Cl4 110.31(5) . . ?
Cl3 Al Cl2 110.63(5) . . ?
Cl4 Al Cl2 110.29(5) . . ?
Cl3 Al Cl1 108.84(4) . . ?
Cl4 Al Cl1 108.95(5) . . ?
Cl2 Al Cl1 107.76(5) . . ?
C1 N1 C5 109.3(2) . . ?
C1 N1 C3 114.8(2) . . ?
C5 N1 C3 113.8(2) . . ?
N1 C1 C2 112.4(2) . . ?
N1 C3 C4 113.4(2) . . ?
C6 C5 N1 112.4(2) . . ?

_refine_diff_density_max         0.350
_refine_diff_density_min         -0.316
_refine_diff_density_rms         0.070


#END

_exptl_crystal_recrystallization_method 'From the Melt'
_chemical_properties_physical    Moisture-sensitive,Hygroscopic
