# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2014

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_[AlCl3(PMe3)]
#data_13jebr06 

_audit_creation_method           'SHELXL-97 + hand edit'
_audit_creation_date             2013-08-18 # yyyy-mm-dd


_chemical_name_systematic        
; 
 trichlorotrimethylphosphanealuminium(III) 
;

# Me3P = C3H9P
# Trimethylphosphine (Chemspider)
# trimethylphosphane (Chemspider)

_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C3 H9 Al Cl3 P'
_chemical_formula_sum            'C3 H9 Al Cl3 P'
_chemical_formula_weight         209.40

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'
Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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_name_H-M_alt        'P 21/m'
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'


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

_cell_length_a                   6.414(3)
_cell_length_b                   10.292(4)
_cell_length_c                   7.649(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 113.698(12)
_cell_angle_gamma                90.00
_cell_volume                     462.4(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    1449
_cell_measurement_theta_min      3.5
_cell_measurement_theta_max      34.6

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.504
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             212
_exptl_absorpt_coefficient_mu    1.174
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.755 # Expt'l Tmin & Tmax 
_exptl_absorpt_correction_T_max  1.000 # scaled to Tmax=1.0 
_exptl_absorpt_process_details   
;Jacobson, R.A. (1998). REQAB. Private communication to the 
 Rigaku Corporation, Tokyo, Japan. 
;


_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  ?
_diffrn_radiation_collimation    'Confocal mirrors, VHF VariMax '

_diffrn_source                   'Rotating anode X-ray tube'
_diffrn_source_type              'Rigaku FR-E+ Superbright'

_diffrn_measurement_device       'Four-circle κ diffractometer'
_diffrn_measurement_device_type  'Rigaku AFC12 '
_diffrn_measurement_method       'Profile data from ω-scans'

_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Rigaku HG Saturn724+ (2x2 bin mode)'
_diffrn_detector_area_resol_mean ?

_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            4220
_diffrn_reflns_av_R_equivalents  0.0562
_diffrn_reflns_av_sigmaI/netI    0.0608
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         3.47
_diffrn_reflns_theta_max         27.48
_reflns_number_total             1113
_reflns_number_gt                1017
_reflns_threshold_expression     I>2σ(I)

_computing_data_collection       'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)'
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'ORTEP-III (Farrugia, 1997)'
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger.

 H atoms on C2 when calculated using AFIX 137 were very close to
 having mirror symmetry. Subsequently these H-atom coordinates were
 calculated to impose m symmetry using DFIXs (C-H, H...H, and H...P)
 and these fixed coordinates used in the final refinement. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0000P)²+2.2858P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         1113
_refine_ls_number_parameters     44
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.0551
_refine_ls_R_factor_gt           0.0519
_refine_ls_wR_factor_ref         0.1250
_refine_ls_wR_factor_gt          0.1241
_refine_ls_goodness_of_fit_ref   1.195
_refine_ls_restrained_S_all      1.190
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Al1 Al 0.5982(3) 0.2500 1.0842(2) 0.0160(4) Uani 1 2 d S . .
Cl1 Cl 0.77960(17) 0.07936(10) 1.21855(15) 0.0212(3) Uani 1 1 d . . .
Cl2 Cl 0.2640(2) 0.2500 1.0795(2) 0.0209(3) Uani 1 2 d S . .
P1 P 0.5707(2) 0.2500 0.7629(2) 0.0146(3) Uani 1 2 d S . .
C1 C 0.7078(7) 0.1091(4) 0.7131(6) 0.0211(9) Uani 1 1 d . . .
H1A H 0.6385 0.0298 0.7366 0.032 Uiso 1 1 calc R . .
H1B H 0.8704 0.1102 0.7964 0.032 Uiso 1 1 calc R . .
H1C H 0.6884 0.1112 0.5793 0.032 Uiso 1 1 calc R . .
C2 C 0.2797(8) 0.2500 0.5887(6) 0.0255(14) Uani 1 2 d S . .
H2A H 0.2785 0.2500 0.4601 0.038 Uiso 1 2 calc S . .
H2B H 0.2014 0.3277 0.6053 0.038 Uiso 0.50 1 calc P . .
H2C H 0.2014 0.1723 0.6053 0.038 Uiso 0.50 1 calc P . .


_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
Al1 Cl1 2.1291(15) 4_565 ?
Al1 Cl1 2.1291(15) . ?
Al1 Cl2 2.130(2) . ?
Al1 P1 2.392(2) . ?
P1 C2 1.806(5) . ?
P1 C1 1.814(4) . ?
P1 C1 1.814(4) 4_565 ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 H2A 0.9806 . ?
C2 H2B 0.9798 . ?
C2 H2C 0.9798 . ?

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 Al1 Cl1 111.15(10) 4_565 . ?
Cl1 Al1 Cl2 111.06(6) 4_565 . ?
Cl1 Al1 Cl2 111.06(6) . . ?
Cl1 Al1 P1 107.22(6) 4_565 . ?
Cl1 Al1 P1 107.22(6) . . ?
Cl2 Al1 P1 108.94(9) . . ?
C2 P1 C1 106.83(16) . . ?
C2 P1 C1 106.83(16) . 4_565 ?
C1 P1 C1 106.1(3) . 4_565 ?
C2 P1 Al1 112.70(14) . . ?
C1 P1 Al1 111.97(15) . . ?
C1 P1 Al1 111.97(15) 4_565 . ?
P1 C1 H1A 109.5 . . ?
P1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
P1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
P1 C2 H2A 109.2 . . ?
P1 C2 H2B 109.6 . . ?
H2A C2 H2B 109.4 . . ?
P1 C2 H2C 109.6 . . ?
H2A C2 H2C 109.4 . . ?
H2B C2 H2C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
# Cl2 Al1 P1 C2 0.000(1) . . . . ? 
Cl1 Al1 P1 C2 -120.28(6) 4_565 . . . ?
Cl1 Al1 P1 C2 120.28(6) . . . . ?
Cl1 Al1 P1 C1 119.25(16) 4_565 . . . ?
Cl1 Al1 P1 C1 -0.19(18) . . . . ?
Cl2 Al1 P1 C1 -120.47(16) . . . . ?
Cl1 Al1 P1 C1 0.19(18) 4_565 . . 4_565 ?
Cl1 Al1 P1 C1 -119.25(16) . . . 4_565 ?
Cl2 Al1 P1 C1 120.47(16) . . . 4_565 ?

_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max         1.087
_refine_diff_density_min         -0.657
_refine_diff_density_rms         0.132

_iucr_refine_instruction_details 
;
 Add final .res file here for Acta Cryst publications or if required.
;
_database_code_depnum_ccdc_archive 'CCDC 1005860'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_[AlCl3(PMe3)2]

#data_13jebr09a 

_audit_creation_method           'SHELXL-97 + hand edit'
_audit_creation_date             2013-08-15 # yyyy-mm-dd

_chemical_name_systematic        
; 
 Trichlorobis(trimethylphosphine)aluminium(III) 
;

# Me3P = C3H9P
# trimethylphosphine (Chemspider)
# trimethylphosphane (Chemspider)

_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C6 H18 Al Cl3 P2'
_chemical_formula_sum            'C6 H18 Al Cl3 P2'
_chemical_formula_weight         285.47

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'
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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_name_H-M_alt        'P n m a'
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'


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

_cell_length_a                   9.970(3)
_cell_length_b                   10.599(4)
_cell_length_c                   13.562(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     1433.1(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    4525
_cell_measurement_theta_min      2.4
_cell_measurement_theta_max      34.5

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.323
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             592
_exptl_absorpt_coefficient_mu    0.883
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.787 # Expt'l Tmin & Tmax 
_exptl_absorpt_correction_T_max  1.000 # scaled to Tmax=1.0 
_exptl_absorpt_process_details   
;Jacobson, R.A. (1998). REQAB. Private communication to the 
 Rigaku Corporation, Tokyo, Japan. 
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  ?
_diffrn_radiation_collimation    'Confocal mirrors, VHF VariMax '

_diffrn_source                   'Rotating anode X-ray tube'
_diffrn_source_type              'Rigaku FR-E+ Superbright'

_diffrn_measurement_device       'Four-circle κ diffractometer'
_diffrn_measurement_device_type  'Rigaku AFC12 '
_diffrn_measurement_method       'Profile data from ω-scans'

_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Rigaku HG Saturn724+ (2x2 bin mode)'
_diffrn_detector_area_resol_mean ?

_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            14433
_diffrn_reflns_av_R_equivalents  0.1398
_diffrn_reflns_av_sigmaI/netI    0.0800
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.18
_diffrn_reflns_theta_max         25.99
_reflns_number_total             1486
_reflns_number_gt                1258
_reflns_threshold_expression     I>2σ(I)

_computing_data_collection       'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)'
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'ORTEP-III (Farrugia, 1997)'
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0000P)²+2.3898P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         1486
_refine_ls_number_parameters     66
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0881
_refine_ls_R_factor_gt           0.0649
_refine_ls_wR_factor_ref         0.0910
_refine_ls_wR_factor_gt          0.0867
_refine_ls_goodness_of_fit_ref   1.191
_refine_ls_restrained_S_all      1.191
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Al1 Al 0.71579(17) 0.2500 0.52181(12) 0.0148(4) Uani 1 2 d S . .
Cl1 Cl 0.78541(9) 0.07226(9) 0.58866(7) 0.0195(2) Uani 1 1 d . . .
Cl2 Cl 0.58038(15) 0.2500 0.39348(11) 0.0238(4) Uani 1 2 d S . .
P1 P 0.51836(15) 0.2500 0.62956(11) 0.0165(4) Uani 1 2 d S . .
P2 P 0.90671(15) 0.2500 0.40700(11) 0.0178(4) Uani 1 2 d S . .
C1 C 0.4102(4) 0.3864(4) 0.6141(3) 0.0278(11) Uani 1 1 d . . .
H1A H 0.3397 0.3851 0.6645 0.042 Uiso 1 1 calc R . .
H1B H 0.3690 0.3841 0.5485 0.042 Uiso 1 1 calc R . .
H1C H 0.4633 0.4637 0.6210 0.042 Uiso 1 1 calc R . .
C2 C 0.5604(6) 0.2500 0.7592(5) 0.0241(14) Uani 1 2 d S . .
H2A H 0.6126 0.1744 0.7748 0.036 Uiso 0.50 1 calc P . .
H2B H 0.4775 0.2500 0.7983 0.036 Uiso 1.00 2 calc S . .
H2C H 0.6126 0.3256 0.7748 0.036 Uiso 0.50 1 calc P . .
C3 C 0.9079(4) 0.1141(4) 0.3262(3) 0.0256(10) Uani 1 1 d . . .
H3A H 0.8250 0.1125 0.2874 0.038 Uiso 1 1 calc R . .
H3B H 0.9141 0.0369 0.3658 0.038 Uiso 1 1 calc R . .
H3C H 0.9852 0.1192 0.2817 0.038 Uiso 1 1 calc R . .
C4 C 1.0717(6) 0.2500 0.4637(5) 0.0249(15) Uani 1 2 d S . .
H4A H 1.0817 0.1746 0.5048 0.037 Uiso 0.50 1 calc P . .
H4B H 1.0817 0.3254 0.5048 0.037 Uiso 0.50 1 calc P . .
H4C H 1.1406 0.2500 0.4120 0.037 Uiso 1.00 2 calc S . .


_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
Al1 Cl2 2.203(2) . ?
Al1 Cl1 2.2029(14) 8_565 ?
Al1 Cl1 2.2029(14) . ?
Al1 P1 2.452(2) . ?
Al1 P2 2.459(2) . ?
P1 C2 1.808(6) . ?
P1 C1 1.816(4) 8_565 ?
P1 C1 1.816(4) . ?
P2 C3 1.810(4) . ?
P2 C3 1.810(4) 8_565 ?
P2 C4 1.816(6) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 H2A 0.9784 . ?
C2 H2B 0.9825 . ?
C2 H2C 0.9784 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 H4A 0.9794 . ?
C4 H4B 0.9794 . ?
C4 H4C 0.9812 . ?

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 Al1 Cl1 121.22(5) . 8_565 ?
Cl2 Al1 Cl1 121.22(5) . . ?
Cl1 Al1 Cl1 117.56(9) 8_565 . ?
Cl2 Al1 P1 88.79(8) . . ?
Cl1 Al1 P1 90.44(6) 8_565 . ?
Cl1 Al1 P1 90.44(6) . . ?
Cl2 Al1 P2 88.52(8) . . ?
Cl1 Al1 P2 90.96(6) 8_565 . ?
Cl1 Al1 P2 90.96(6) . . ?
P1 Al1 P2 177.31(9) . . ?
C2 P1 C1 104.48(19) . 8_565 ?
C2 P1 C1 104.48(19) . . ?
C1 P1 C1 105.5(3) 8_565 . ?
C2 P1 Al1 113.2(2) . . ?
C1 P1 Al1 114.09(15) 8_565 . ?
C1 P1 Al1 114.09(15) . . ?
C3 P2 C3 105.5(3) . 8_565 ?
C3 P2 C4 104.50(19) . . ?
C3 P2 C4 104.50(19) 8_565 . ?
C3 P2 Al1 112.85(15) . . ?
C3 P2 Al1 112.85(15) 8_565 . ?
C4 P2 Al1 115.7(2) . . ?
P1 C1 H1A 109.5 . . ?
P1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
P1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
P1 C2 H2A 109.5 . . ?
P1 C2 H2B 109.3 . . ?
H2A C2 H2B 109.3 . . ?
P1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.9 . . ?
H2B C2 H2C 109.3 . . ?
P2 C3 H3A 109.5 . . ?
P2 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
P2 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
P2 C4 H4A 109.4 . . ?
P2 C4 H4B 109.4 . . ?
H4A C4 H4B 109.5 . . ?
P2 C4 H4C 109.3 . . ?
H4A C4 H4C 109.6 . . ?
H4B C4 H4C 109.6 . . ?

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
# P2 Al1 P1 C2 180.000(3) . . . . ? 
# P2 Al1 P1 C1 60.71(17) . . . 8_565 ? 
# P2 Al1 P1 C1 -60.71(17) . . . . ? 
# P1 Al1 P2 C3 -59.74(16) . . . . ? 
# P1 Al1 P2 C3 59.74(16) . . . 8_565 ? 
Cl2 Al1 P1 C2 180.0 . . . . ?
Cl1 Al1 P1 C2 -58.78(5) 8_565 . . . ?
Cl1 Al1 P1 C2 58.78(5) . . . . ?
Cl2 Al1 P1 C1 60.71(17) . . . 8_565 ?
Cl1 Al1 P1 C1 -178.07(17) 8_565 . . 8_565 ?
Cl1 Al1 P1 C1 -60.51(18) . . . 8_565 ?
Cl2 Al1 P1 C1 -60.71(17) . . . . ?
Cl1 Al1 P1 C1 60.51(18) 8_565 . . . ?
Cl1 Al1 P1 C1 178.07(17) . . . . ?
Cl2 Al1 P2 C3 -59.74(16) . . . . ?
Cl1 Al1 P2 C3 179.06(16) 8_565 . . . ?
Cl1 Al1 P2 C3 61.47(17) . . . . ?
Cl2 Al1 P2 C3 59.74(16) . . . 8_565 ?
Cl1 Al1 P2 C3 -61.47(17) 8_565 . . 8_565 ?
Cl1 Al1 P2 C3 -179.06(17) . . . 8_565 ?
Cl2 Al1 P2 C4 180.0 . . . . ?
Cl1 Al1 P2 C4 58.79(5) 8_565 . . . ?
Cl1 Al1 P2 C4 -58.79(5) . . . . ?
# P1 Al1 P2 C4 180.000(4) . . . . ? 

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        25.99
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.613
_refine_diff_density_min         -0.713
_refine_diff_density_rms         0.198

_iucr_refine_instruction_details 
;
 Add final .res file here for Acta Cryst publications or if required.
;
_database_code_depnum_ccdc_archive 'CCDC 1005861'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_[AlCl2{o-C6H4(PMe2)2}2][AlCl4]
#data_13jebr14 

_audit_creation_method           'SHELXL-97 + hand edit'
_audit_creation_date             2013-08-15 # yyyy-mm-dd

_chemical_name_systematic        
; 
 dichlorobis(1,2-bis(dimethylphosphino)benzene)aluminium(III)
 tetrachloroaluminate  
;

# o-C6H4(PMe2)2 = C10H16P2 = diphos
# 1,2-bis(dimethylphosphino)benzene 
# 1,2-phenylenebis(dimethylphosphine)    (iLab name (defaults))
# benzene-1,2-diylbis(dimethylphosphane) (iLab name (selected options))
# (2-dimethylphosphanylphenyl)-dimethyl-phosphane  (Chemspider)
# 1,2-bis(dimethylphosphanyl)benzene
# o-phenylenebis(dimethylphosphine)

_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C20 H32 Al Cl2 P4 1+, Al Cl4 1-'
_chemical_formula_sum            'C20 H32 Al2 Cl6 P4'
_chemical_formula_weight         663.00

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'
Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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_name_H-M_alt        'C 2/c'
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'

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

_cell_length_a                   13.278(4)
_cell_length_b                   14.545(4)
_cell_length_c                   16.554(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 104.126(6)
_cell_angle_gamma                90.00
_cell_volume                     3100.2(16)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    5045
_cell_measurement_theta_min      2.1
_cell_measurement_theta_max      34.9

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.420
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1360
_exptl_absorpt_coefficient_mu    0.828
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.902 # Expt'l Tmin & Tmax
_exptl_absorpt_correction_T_max  1.000 # scaled to Tmax=1.0 
_exptl_absorpt_process_details   
;Jacobson, R.A. (1998). REQAB. Private communication to the 
 Rigaku Corporation, Tokyo, Japan. 
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  ?
_diffrn_radiation_collimation    'Confocal mirrors, VHF VariMax '

_diffrn_source                   'Rotating anode X-ray tube'
_diffrn_source_type              'Rigaku FR-E+ Superbright'

_diffrn_measurement_device       'Four-circle κ diffractometer'
_diffrn_measurement_device_type  'Rigaku AFC12 '
_diffrn_measurement_method       'Profile data from ω-scans'

_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Rigaku HG Saturn724+ (2x2 bin mode)'
_diffrn_detector_area_resol_mean ?

_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            14366
_diffrn_reflns_av_R_equivalents  0.0321
# _diffrn_reflns_av_sigmaI/netI   0.0301
_diffrn_reflns_av_unetI/netI     0.0301
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         3.59
_diffrn_reflns_theta_max         27.49
_reflns_number_total             3544
_reflns_number_gt                3257
_reflns_threshold_expression     I>2σ(I)

_computing_data_collection       'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)'
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'ORTEP-III (Farrugia, 1997)'
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0273P)²+2.1045P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3544
_refine_ls_number_parameters     151
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0352
_refine_ls_R_factor_gt           0.0300
_refine_ls_wR_factor_ref         0.0671
_refine_ls_wR_factor_gt          0.0648
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_restrained_S_all      1.079
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Al1 Al 0.0000 0.0000 0.5000 0.01254(14) Uani 1 2 d S . .
Al2 Al 0.5000 0.09156(5) 0.2500 0.01405(15) Uani 1 2 d S . .
Cl1 Cl -0.10981(3) 0.00369(3) 0.37134(2) 0.01713(10) Uani 1 1 d . . .
Cl2 Cl 0.62342(3) 0.17541(3) 0.31837(3) 0.02407(11) Uani 1 1 d . . .
Cl3 Cl 0.44371(4) 0.00795(3) 0.33593(3) 0.02289(11) Uani 1 1 d . . .
P1 P 0.00828(3) 0.16971(3) 0.49333(3) 0.01355(10) Uani 1 1 d . . .
P2 P 0.14509(3) 0.01379(3) 0.43032(3) 0.01329(10) Uani 1 1 d . . .
C1 C 0.07535(12) 0.19596(11) 0.41230(10) 0.0145(3) Uani 1 1 d . . .
C2 C 0.13188(12) 0.12759(11) 0.38252(10) 0.0142(3) Uani 1 1 d . . .
C3 C 0.17983(13) 0.14896(12) 0.31825(10) 0.0175(3) Uani 1 1 d . . .
H3 H 0.2170 0.1028 0.2970 0.021 Uiso 1 1 calc R . .
C4 C 0.17321(13) 0.23701(12) 0.28552(10) 0.0197(4) Uani 1 1 d . . .
H4 H 0.2053 0.2508 0.2415 0.024 Uiso 1 1 calc R . .
C5 C 0.12007(13) 0.30514(12) 0.31657(11) 0.0203(4) Uani 1 1 d . . .
H5 H 0.1172 0.3658 0.2949 0.024 Uiso 1 1 calc R . .
C6 C 0.07106(13) 0.28452(12) 0.37936(11) 0.0188(3) Uani 1 1 d . . .
H6 H 0.0342 0.3312 0.4001 0.023 Uiso 1 1 calc R . .
C7 C 0.08178(14) 0.23081(12) 0.58418(11) 0.0218(4) Uani 1 1 d . . .
H7A H 0.1531 0.2072 0.5995 0.033 Uiso 1 1 calc R . .
H7B H 0.0492 0.2217 0.6307 0.033 Uiso 1 1 calc R . .
H7C H 0.0828 0.2966 0.5715 0.033 Uiso 1 1 calc R . .
C8 C -0.11541(13) 0.22993(12) 0.46320(11) 0.0211(4) Uani 1 1 d . . .
H8A H -0.1509 0.2261 0.5085 0.032 Uiso 1 1 calc R . .
H8B H -0.1587 0.2015 0.4129 0.032 Uiso 1 1 calc R . .
H8C H -0.1032 0.2946 0.4519 0.032 Uiso 1 1 calc R . .
C9 C 0.14939(14) -0.06631(12) 0.34726(11) 0.0214(4) Uani 1 1 d . . .
H9A H 0.0845 -0.0623 0.3038 0.032 Uiso 1 1 calc R . .
H9B H 0.1580 -0.1290 0.3696 0.032 Uiso 1 1 calc R . .
H9C H 0.2080 -0.0509 0.3234 0.032 Uiso 1 1 calc R . .
C10 C 0.27634(13) 0.01267(12) 0.49704(11) 0.0202(4) Uani 1 1 d . . .
H10A H 0.2909 -0.0478 0.5234 0.030 Uiso 1 1 calc R . .
H10B H 0.2826 0.0600 0.5401 0.030 Uiso 1 1 calc R . .
H10C H 0.3262 0.0252 0.4635 0.030 Uiso 1 1 calc R . .


_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
Al1 Cl1 2.2692(7) 5_556 ?
Al1 Cl1 2.2692(7) . ?
Al1 P1 2.4745(8) . ?
Al1 P1 2.4745(8) 5_556 ?
Al1 P2 2.4832(7) . ?
Al1 P2 2.4832(7) 5_556 ?
Al2 Cl2 2.1327(7) . ?
Al2 Cl2 2.1327(7) 2_655 ?
Al2 Cl3 2.1401(7) . ?
Al2 Cl3 2.1401(7) 2_655 ?
P1 C7 1.8131(18) . ?
P1 C8 1.8203(17) . ?
P1 C1 1.8223(17) . ?
P2 C9 1.8138(17) . ?
P2 C10 1.8215(18) . ?
P2 C2 1.8245(17) . ?
C1 C6 1.395(2) . ?
C1 C2 1.406(2) . ?
C2 C3 1.402(2) . ?
C3 C4 1.385(2) . ?
C3 H3 0.9500 . ?
C4 C5 1.386(2) . ?
C4 H4 0.9500 . ?
C5 C6 1.387(2) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?

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 Al1 Cl1 180.0 5_556 . ?
Cl1 Al1 P1 92.297(14) 5_556 . ?
Cl1 Al1 P1 87.703(14) . . ?
Cl1 Al1 P1 87.703(14) 5_556 5_556 ?
Cl1 Al1 P1 92.297(14) . 5_556 ?
P1 Al1 P1 180.0 . 5_556 ?
Cl1 Al1 P2 92.54(3) 5_556 . ?
Cl1 Al1 P2 87.46(3) . . ?
P1 Al1 P2 81.415(13) . . ?
P1 Al1 P2 98.585(13) 5_556 . ?
Cl1 Al1 P2 87.46(3) 5_556 5_556 ?
Cl1 Al1 P2 92.54(3) . 5_556 ?
P1 Al1 P2 98.585(13) . 5_556 ?
P1 Al1 P2 81.415(13) 5_556 5_556 ?
P2 Al1 P2 180.0 . 5_556 ?
Cl2 Al2 Cl2 110.25(4) . 2_655 ?
Cl2 Al2 Cl3 108.66(3) . . ?
Cl2 Al2 Cl3 109.26(2) 2_655 . ?
Cl2 Al2 Cl3 109.26(3) . 2_655 ?
Cl2 Al2 Cl3 108.66(3) 2_655 2_655 ?
Cl3 Al2 Cl3 110.74(4) . 2_655 ?
C7 P1 C8 104.97(9) . . ?
C7 P1 C1 104.31(8) . . ?
C8 P1 C1 105.54(8) . . ?
C7 P1 Al1 118.21(6) . . ?
C8 P1 Al1 116.44(6) . . ?
C1 P1 Al1 106.07(5) . . ?
C9 P2 C10 104.57(9) . . ?
C9 P2 C2 105.75(8) . . ?
C10 P2 C2 104.33(8) . . ?
C9 P2 Al1 118.15(6) . . ?
C10 P2 Al1 116.97(6) . . ?
C2 P2 Al1 105.75(5) . . ?
C6 C1 C2 119.38(15) . . ?
C6 C1 P1 120.04(13) . . ?
C2 C1 P1 120.58(12) . . ?
C3 C2 C1 119.33(15) . . ?
C3 C2 P2 121.13(13) . . ?
C1 C2 P2 119.52(12) . . ?
C4 C3 C2 120.32(16) . . ?
C4 C3 H3 119.8 . . ?
C2 C3 H3 119.8 . . ?
C3 C4 C5 120.36(16) . . ?
C3 C4 H4 119.8 . . ?
C5 C4 H4 119.8 . . ?
C4 C5 C6 119.85(16) . . ?
C4 C5 H5 120.1 . . ?
C6 C5 H5 120.1 . . ?
C5 C6 C1 120.72(16) . . ?
C5 C6 H6 119.6 . . ?
C1 C6 H6 119.6 . . ?
P1 C7 H7A 109.5 . . ?
P1 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
P1 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
P1 C8 H8A 109.5 . . ?
P1 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
P1 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
P2 C9 H9A 109.5 . . ?
P2 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
P2 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
P2 C10 H10A 109.5 . . ?
P2 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
P2 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C7 P1 C1 C6 -69.79(15) . . . . ?
C8 P1 C1 C6 40.55(15) . . . . ?
Al1 P1 C1 C6 164.67(12) . . . . ?
C7 P1 C1 C2 110.09(14) . . . . ?
C8 P1 C1 C2 -139.56(13) . . . . ?
Al1 P1 C1 C2 -15.44(14) . . . . ?
C6 C1 C2 C3 -2.2(2) . . . . ?
P1 C1 C2 C3 177.91(12) . . . . ?
C6 C1 C2 P2 175.84(12) . . . . ?
P1 C1 C2 P2 -4.04(18) . . . . ?
C9 P2 C2 C3 -34.68(15) . . . . ?
C10 P2 C2 C3 75.31(15) . . . . ?
Al1 P2 C2 C3 -160.75(12) . . . . ?
C9 P2 C2 C1 147.31(13) . . . . ?
C10 P2 C2 C1 -102.71(14) . . . . ?
Al1 P2 C2 C1 21.24(13) . . . . ?
C1 C2 C3 C4 1.2(2) . . . . ?
P2 C2 C3 C4 -176.80(12) . . . . ?
C2 C3 C4 C5 0.7(2) . . . . ?
C3 C4 C5 C6 -1.6(3) . . . . ?
C4 C5 C6 C1 0.6(3) . . . . ?
C2 C1 C6 C5 1.3(2) . . . . ?
P1 C1 C6 C5 -178.79(13) . . . . ?


_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        27.49
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         0.419
_refine_diff_density_min         -0.226
_refine_diff_density_rms         0.057

_iucr_refine_instruction_details 
;
 Add final .res file here for Acta Cryst publications or if required.
;
_database_code_depnum_ccdc_archive 'CCDC 1005862'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_[AlCl2{o-C6H4(PPh2)2}2][AlCl4]
#data_13jebr21 

_audit_creation_method           'SHELXL-97 + hand edit'
_audit_creation_date             2013-09-11 # yyyy-mm-dd

_chemical_name_systematic        
; 
 bis(benzene-1,2-diylbis(diphenylphosphane))dichloroaluminium(III)
 tetrachloroaluminate 
;

# o-C6H4(PPh2)2 = C30H24P2
# benzene-1,2-diylbis(diphenylphosphane)  (iLab name (selected options))  
# 1,2-phenylenebis(diphenylphosphine)     (iLab defaults) 
# benzene-1,2-diylbis(diphenylphosphane)  (ACD I-Lab 2.0 defaults)
# 1,2-bis(diphenylphosphanyl)benzene 
# 1,2-bis(diphenylphosphino)benzene
# o-phenylenebis(diphenylphosphine) 


_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C60 H48 Al Cl2 P4 1+, Al Cl4 1-'
_chemical_formula_sum            'C60 H48 Al2 Cl6 P4'
_chemical_formula_structural     '((C30 H24 P2)2 Al Cl2) (Al Cl4)'
_chemical_formula_weight         1159.52

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'
Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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      triclinic
_space_group_name_H-M_alt        'P -1'
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.024(3)
_cell_length_b                   11.752(4)
_cell_length_c                   24.434(8)
_cell_angle_alpha                81.926(14)
_cell_angle_beta                 85.52(2)
_cell_angle_gamma                82.25(2)
_cell_volume                     2818.9(16)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    7440
_cell_measurement_theta_min      2.1
_cell_measurement_theta_max      34.6

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.366
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1192
_exptl_absorpt_coefficient_mu    0.489
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.817 # Expt'l Tmin & Tmax
_exptl_absorpt_correction_T_max  1.000 # scaled to Tmax=1.0 
_exptl_absorpt_process_details   
;Jacobson, R.A. (1998). REQAB. Private communication to the 
 Rigaku Corporation, Tokyo, Japan. 
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  ?
_diffrn_radiation_collimation    'Confocal mirrors, VHF VariMax '

_diffrn_source                   'Rotating anode X-ray tube'
_diffrn_source_type              'Rigaku FR-E+ Superbright'

_diffrn_measurement_device       'Four-circle κ diffractometer'
_diffrn_measurement_device_type  'Rigaku AFC12 '
_diffrn_measurement_method       'Profile data from ω-scans'

_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Rigaku HG Saturn724+ (2x2 bin mode)'
_diffrn_detector_area_resol_mean ?

_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            24430
_diffrn_reflns_av_R_equivalents  0.0757
# _diffrn_reflns_av_sigmaI/netI   0.1460 
_diffrn_reflns_av_unetI/netI     0.1460
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_theta_min         2.96
_diffrn_reflns_theta_max         27.48
_reflns_number_total             12194
_reflns_number_gt                7266
_reflns_threshold_expression     I>2σ(I)

_computing_data_collection       'CrystalClear-SM Expert 2.0 r13 (Rigaku, 2011)'
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r13 (Rigaku, 2011)'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 r13 (Rigaku, 2011)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'ORTEP-III (Farrugia, 1997)'
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 

 _diffrn_measured_fraction_theta_full Low (0.943) this was due to a 
 sub-optimal data collection strategy  
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0595P)²+0.5098P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         12194
_refine_ls_number_parameters     652
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1354
_refine_ls_R_factor_gt           0.0793
_refine_ls_wR_factor_ref         0.1934
_refine_ls_wR_factor_gt          0.1594
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_restrained_S_all      1.081
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Al1 Al 1.0000 0.5000 0.5000 0.0163(4) Uani 1 2 d S . .
Al2 Al 0.0000 0.5000 0.0000 0.0238(5) Uani 1 2 d S . .
Al3 Al 0.45780(17) 0.02216(14) 0.23755(6) 0.0300(4) Uani 1 1 d . . .
Cl1 Cl 0.79431(11) 0.55162(10) 0.46981(5) 0.0198(3) Uani 1 1 d . . .
Cl2 Cl -0.20506(13) 0.57575(11) -0.02602(5) 0.0274(3) Uani 1 1 d . . .
Cl3 Cl 0.62500(14) 0.05173(13) 0.28077(6) 0.0380(4) Uani 1 1 d . . .
Cl4 Cl 0.45606(18) -0.15936(13) 0.23864(7) 0.0519(5) Uani 1 1 d . . .
Cl5 Cl 0.47780(15) 0.10620(13) 0.15420(5) 0.0377(4) Uani 1 1 d . . .
Cl6 Cl 0.27594(14) 0.09376(13) 0.27840(6) 0.0373(4) Uani 1 1 d . . .
P1 P 0.96801(12) 0.28997(10) 0.49398(5) 0.0172(3) Uani 1 1 d . . .
P2 P 1.08240(13) 0.48125(11) 0.39839(5) 0.0179(3) Uani 1 1 d . . .
P3 P -0.07189(14) 0.54798(12) 0.09763(5) 0.0260(3) Uani 1 1 d . . .
P4 P 0.04661(14) 0.71025(12) -0.00591(5) 0.0249(3) Uani 1 1 d . . .
C1 C 1.1049(5) 0.1798(4) 0.51743(19) 0.0184(10) Uani 1 1 d . . .
C2 C 1.1399(5) 0.1715(4) 0.57215(19) 0.0226(11) Uani 1 1 d . . .
H2 H 1.0905 0.2208 0.5963 0.027 Uiso 1 1 calc R . .
C3 C 1.2461(5) 0.0920(4) 0.5916(2) 0.0231(11) Uani 1 1 d . . .
H3 H 1.2665 0.0844 0.6293 0.028 Uiso 1 1 calc R . .
C4 C 1.3230(5) 0.0233(4) 0.5557(2) 0.0275(12) Uani 1 1 d . . .
H4 H 1.3965 -0.0307 0.5688 0.033 Uiso 1 1 calc R . .
C5 C 1.2917(5) 0.0341(4) 0.5009(2) 0.0274(12) Uani 1 1 d . . .
H5 H 1.3443 -0.0123 0.4763 0.033 Uiso 1 1 calc R . .
C6 C 1.1844(5) 0.1119(4) 0.4818(2) 0.0212(11) Uani 1 1 d . . .
H6 H 1.1644 0.1194 0.4440 0.025 Uiso 1 1 calc R . .
C7 C 0.8093(5) 0.2424(4) 0.52630(19) 0.0208(11) Uani 1 1 d . . .
C8 C 0.8051(5) 0.1748(4) 0.57792(19) 0.0243(11) Uani 1 1 d . . .
H8 H 0.8863 0.1411 0.5945 0.029 Uiso 1 1 calc R . .
C9 C 0.6801(5) 0.1571(5) 0.6049(2) 0.0305(13) Uani 1 1 d . . .
H9 H 0.6764 0.1119 0.6403 0.037 Uiso 1 1 calc R . .
C10 C 0.5626(5) 0.2044(5) 0.5808(2) 0.0317(13) Uani 1 1 d . . .
H10 H 0.4785 0.1951 0.6005 0.038 Uiso 1 1 calc R . .
C11 C 0.5652(5) 0.2661(4) 0.5277(2) 0.0297(12) Uani 1 1 d . . .
H11 H 0.4839 0.2936 0.5100 0.036 Uiso 1 1 calc R . .
C12 C 0.6906(5) 0.2865(4) 0.5011(2) 0.0227(11) Uani 1 1 d . . .
H12 H 0.6941 0.3310 0.4655 0.027 Uiso 1 1 calc R . .
C13 C 0.9584(5) 0.2768(4) 0.42061(19) 0.0193(10) Uani 1 1 d . . .
C14 C 0.9091(5) 0.1823(4) 0.4052(2) 0.0210(11) Uani 1 1 d . . .
H14 H 0.8758 0.1265 0.4330 0.025 Uiso 1 1 calc R . .
C15 C 0.9073(5) 0.1670(4) 0.35022(19) 0.0249(11) Uani 1 1 d . . .
H15 H 0.8739 0.1014 0.3402 0.030 Uiso 1 1 calc R . .
C16 C 0.9559(5) 0.2505(4) 0.3093(2) 0.0236(11) Uani 1 1 d . . .
H16 H 0.9554 0.2413 0.2713 0.028 Uiso 1 1 calc R . .
C17 C 1.0044(5) 0.3460(4) 0.32408(19) 0.0216(11) Uani 1 1 d . . .
H17 H 1.0358 0.4023 0.2960 0.026 Uiso 1 1 calc R . .
C18 C 1.0076(5) 0.3605(4) 0.37979(19) 0.0179(10) Uani 1 1 d . . .
C19 C 1.2637(5) 0.4428(4) 0.38350(18) 0.0203(10) Uani 1 1 d . . .
C20 C 1.3514(5) 0.5144(4) 0.39798(19) 0.0229(11) Uani 1 1 d . . .
H20 H 1.3162 0.5815 0.4145 0.027 Uiso 1 1 calc R . .
C21 C 1.4904(5) 0.4884(5) 0.3884(2) 0.0299(12) Uani 1 1 d . . .
H21 H 1.5497 0.5380 0.3980 0.036 Uiso 1 1 calc R . .
C22 C 1.5412(6) 0.3900(5) 0.3649(2) 0.0339(13) Uani 1 1 d . . .
H22 H 1.6358 0.3727 0.3579 0.041 Uiso 1 1 calc R . .
C23 C 1.4553(5) 0.3161(5) 0.3514(2) 0.0327(13) Uani 1 1 d . . .
H23 H 1.4912 0.2478 0.3359 0.039 Uiso 1 1 calc R . .
C24 C 1.3169(5) 0.3424(4) 0.36072(19) 0.0246(11) Uani 1 1 d . . .
H24 H 1.2581 0.2919 0.3516 0.029 Uiso 1 1 calc R . .
C25 C 1.0246(5) 0.6021(4) 0.34551(18) 0.0217(11) Uani 1 1 d . . .
C26 C 0.8896(5) 0.6171(4) 0.33186(19) 0.0246(11) Uani 1 1 d . . .
H26 H 0.8316 0.5617 0.3472 0.030 Uiso 1 1 calc R . .
C27 C 0.8412(5) 0.7127(5) 0.2960(2) 0.0299(12) Uani 1 1 d . . .
H27 H 0.7503 0.7218 0.2860 0.036 Uiso 1 1 calc R . .
C28 C 0.9245(6) 0.7956(5) 0.2744(2) 0.0333(13) Uani 1 1 d . . .
H28 H 0.8901 0.8620 0.2504 0.040 Uiso 1 1 calc R . .
C29 C 1.0567(6) 0.7813(4) 0.2879(2) 0.0305(13) Uani 1 1 d . . .
H29 H 1.1138 0.8376 0.2727 0.037 Uiso 1 1 calc R . .
C30 C 1.1077(5) 0.6850(4) 0.32355(19) 0.0230(11) Uani 1 1 d . . .
H30 H 1.1991 0.6760 0.3329 0.028 Uiso 1 1 calc R . .
C31 C -0.2109(5) 0.4831(5) 0.1377(2) 0.0281(12) Uani 1 1 d . . .
C32 C -0.1985(6) 0.4275(5) 0.1909(2) 0.0339(13) Uani 1 1 d . . .
H32 H -0.1179 0.4272 0.2089 0.041 Uiso 1 1 calc R . .
C33 C -0.3034(6) 0.3716(5) 0.2183(2) 0.0368(14) Uani 1 1 d . . .
H33 H -0.2943 0.3338 0.2551 0.044 Uiso 1 1 calc R . .
C34 C -0.4196(6) 0.3710(5) 0.1924(2) 0.0404(15) Uani 1 1 d . . .
H34 H -0.4893 0.3297 0.2105 0.048 Uiso 1 1 calc R . .
C35 C -0.4356(6) 0.4307(5) 0.1397(2) 0.0429(15) Uani 1 1 d . . .
H35 H -0.5175 0.4328 0.1222 0.051 Uiso 1 1 calc R . .
C36 C -0.3325(6) 0.4867(5) 0.1127(2) 0.0357(14) Uani 1 1 d . . .
H36 H -0.3439 0.5283 0.0768 0.043 Uiso 1 1 calc R . .
C37 C 0.0627(5) 0.5317(5) 0.1444(2) 0.0289(12) Uani 1 1 d . . .
C38 C 0.1083(6) 0.6279(5) 0.1616(2) 0.0318(13) Uani 1 1 d . . .
H38 H 0.0670 0.7039 0.1494 0.038 Uiso 1 1 calc R . .
C39 C 0.2150(6) 0.6114(5) 0.1968(2) 0.0401(15) Uani 1 1 d . . .
H39 H 0.2498 0.6765 0.2067 0.048 Uiso 1 1 calc R . .
C40 C 0.2693(6) 0.5016(5) 0.2170(2) 0.0351(14) Uani 1 1 d . . .
H40 H 0.3389 0.4911 0.2422 0.042 Uiso 1 1 calc R . .
C41 C 0.2238(5) 0.4057(5) 0.2011(2) 0.0339(14) Uani 1 1 d . . .
H41 H 0.2612 0.3298 0.2156 0.041 Uiso 1 1 calc R . .
C42 C 0.1229(5) 0.4212(5) 0.1636(2) 0.0309(13) Uani 1 1 d . . .
H42 H 0.0951 0.3557 0.1511 0.037 Uiso 1 1 calc R . .
C43 C -0.1304(5) 0.7031(4) 0.0879(2) 0.0263(12) Uani 1 1 d . . .
C44 C -0.2240(6) 0.7520(5) 0.1268(2) 0.0326(13) Uani 1 1 d . . .
H44 H -0.2558 0.7047 0.1586 0.039 Uiso 1 1 calc R . .
C45 C -0.2695(6) 0.8690(5) 0.1184(2) 0.0385(14) Uani 1 1 d . . .
H45 H -0.3308 0.9021 0.1452 0.046 Uiso 1 1 calc R . .
C46 C -0.2273(6) 0.9390(5) 0.0715(2) 0.0347(14) Uani 1 1 d . . .
H46 H -0.2622 1.0186 0.0653 0.042 Uiso 1 1 calc R . .
C47 C -0.1343(5) 0.8914(4) 0.0341(2) 0.0306(13) Uani 1 1 d . . .
H47 H -0.1039 0.9399 0.0024 0.037 Uiso 1 1 calc R . .
C48 C -0.0830(5) 0.7744(4) 0.0412(2) 0.0260(12) Uani 1 1 d . . .
C49 C 0.2031(5) 0.7476(5) 0.0164(2) 0.0288(12) Uani 1 1 d . . .
C50 C 0.2042(6) 0.8318(5) 0.0517(2) 0.0384(14) Uani 1 1 d . . .
H50 H 0.1217 0.8681 0.0667 0.046 Uiso 1 1 calc R . .
C51 C 0.3252(7) 0.8618(6) 0.0645(3) 0.0530(18) Uani 1 1 d . . .
H51 H 0.3259 0.9195 0.0881 0.064 Uiso 1 1 calc R . .
C52 C 0.4473(7) 0.8073(6) 0.0429(3) 0.0533(18) Uani 1 1 d . . .
H52 H 0.5304 0.8286 0.0516 0.064 Uiso 1 1 calc R . .
C53 C 0.4469(6) 0.7230(6) 0.0091(3) 0.0508(18) Uani 1 1 d . . .
H53 H 0.5295 0.6862 -0.0055 0.061 Uiso 1 1 calc R . .
C54 C 0.3233(6) 0.6917(5) -0.0036(2) 0.0405(15) Uani 1 1 d . . .
H54 H 0.3227 0.6320 -0.0261 0.049 Uiso 1 1 calc R . .
C55 C 0.0252(6) 0.7964(4) -0.0739(2) 0.0282(12) Uani 1 1 d . . .
C56 C -0.1026(5) 0.8382(4) -0.0925(2) 0.0280(12) Uani 1 1 d . . .
H56 H -0.1805 0.8251 -0.0690 0.034 Uiso 1 1 calc R . .
C57 C -0.1167(6) 0.8985(5) -0.1450(2) 0.0373(14) Uani 1 1 d . . .
H57 H -0.2040 0.9274 -0.1572 0.045 Uiso 1 1 calc R . .
C58 C -0.0027(6) 0.9168(5) -0.1800(2) 0.0343(14) Uani 1 1 d . . .
H58 H -0.0121 0.9606 -0.2155 0.041 Uiso 1 1 calc R . .
C59 C 0.1228(6) 0.8717(5) -0.1630(2) 0.0346(14) Uani 1 1 d . . .
H59 H 0.1998 0.8812 -0.1877 0.041 Uiso 1 1 calc R . .
C60 C 0.1386(5) 0.8120(4) -0.1101(2) 0.0289(12) Uani 1 1 d . . .
H60 H 0.2262 0.7819 -0.0986 0.035 Uiso 1 1 calc R . .


_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
Al1 Cl1 2.2222(13) . ?
Al1 Cl1 2.2222(13) 2_766 ?
Al1 P1 2.5574(15) . ?
Al1 P1 2.5574(15) 2_766 ?
Al1 P2 2.5843(15) . ?
Al1 P2 2.5843(15) 2_766 ?
Al2 Cl2 2.2302(14) . ?
Al2 Cl2 2.2302(14) 2_565 ?
Al2 P3 2.5549(15) 2_565 ?
Al2 P3 2.5549(16) . ?
Al2 P4 2.5584(16) 2_565 ?
Al2 P4 2.5584(16) . ?
Al3 Cl4 2.132(2) . ?
Al3 Cl6 2.137(2) . ?
Al3 Cl3 2.141(2) . ?
Al3 Cl5 2.142(2) . ?
P1 C1 1.823(5) . ?
P1 C13 1.832(5) . ?
P1 C7 1.841(5) . ?
P2 C18 1.818(5) . ?
P2 C19 1.833(5) . ?
P2 C25 1.844(5) . ?
P3 C37 1.809(6) . ?
P3 C43 1.826(5) . ?
P3 C31 1.829(5) . ?
P4 C48 1.824(5) . ?
P4 C49 1.827(5) . ?
P4 C55 1.831(5) . ?
C1 C6 1.393(6) . ?
C1 C2 1.396(6) . ?
C2 C3 1.384(6) . ?
C2 H2 0.9500 . ?
C3 C4 1.393(7) . ?
C3 H3 0.9500 . ?
C4 C5 1.384(7) . ?
C4 H4 0.9500 . ?
C5 C6 1.380(7) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 C12 1.387(6) . ?
C7 C8 1.394(6) . ?
C8 C9 1.397(7) . ?
C8 H8 0.9500 . ?
C9 C10 1.372(7) . ?
C9 H9 0.9500 . ?
C10 C11 1.394(7) . ?
C10 H10 0.9500 . ?
C11 C12 1.404(6) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
C13 C14 1.384(6) . ?
C13 C18 1.409(6) . ?
C14 C15 1.381(6) . ?
C14 H14 0.9500 . ?
C15 C16 1.405(6) . ?
C15 H15 0.9500 . ?
C16 C17 1.383(6) . ?
C16 H16 0.9500 . ?
C17 C18 1.399(6) . ?
C17 H17 0.9500 . ?
C19 C24 1.398(7) . ?
C19 C20 1.392(7) . ?
C20 C21 1.394(7) . ?
C20 H20 0.9500 . ?
C21 C22 1.381(7) . ?
C21 H21 0.9500 . ?
C22 C23 1.390(8) . ?
C22 H22 0.9500 . ?
C23 C24 1.388(7) . ?
C23 H23 0.9500 . ?
C24 H24 0.9500 . ?
C25 C30 1.390(6) . ?
C25 C26 1.402(7) . ?
C26 C27 1.381(6) . ?
C26 H26 0.9500 . ?
C27 C28 1.390(7) . ?
C27 H27 0.9500 . ?
C28 C29 1.373(7) . ?
C28 H28 0.9500 . ?
C29 C30 1.392(6) . ?
C29 H29 0.9500 . ?
C30 H30 0.9500 . ?
C31 C32 1.377(7) . ?
C31 C36 1.398(7) . ?
C32 C33 1.392(7) . ?
C32 H32 0.9500 . ?
C33 C34 1.371(8) . ?
C33 H33 0.9500 . ?
C34 C35 1.387(8) . ?
C34 H34 0.9500 . ?
C35 C36 1.376(7) . ?
C35 H35 0.9500 . ?
C36 H36 0.9500 . ?
C37 C42 1.390(7) . ?
C37 C38 1.401(7) . ?
C38 C39 1.401(7) . ?
C38 H38 0.9500 . ?
C39 C40 1.371(8) . ?
C39 H39 0.9500 . ?
C40 C41 1.385(8) . ?
C40 H40 0.9500 . ?
C41 C42 1.394(7) . ?
C41 H41 0.9500 . ?
C42 H42 0.9500 . ?
C43 C44 1.408(7) . ?
C43 C48 1.409(6) . ?
C44 C45 1.381(7) . ?
C44 H44 0.9500 . ?
C45 C46 1.387(7) . ?
C45 H45 0.9500 . ?
C46 C47 1.373(7) . ?
C46 H46 0.9500 . ?
C47 C48 1.394(7) . ?
C47 H47 0.9500 . ?
C49 C54 1.382(7) . ?
C49 C50 1.403(7) . ?
C50 C51 1.378(8) . ?
C50 H50 0.9500 . ?
C51 C52 1.404(9) . ?
C51 H51 0.9500 . ?
C52 C53 1.376(9) . ?
C52 H52 0.9500 . ?
C53 C54 1.408(8) . ?
C53 H53 0.9500 . ?
C54 H54 0.9500 . ?
C55 C56 1.396(7) . ?
C55 C60 1.401(7) . ?
C56 C57 1.382(7) . ?
C56 H56 0.9500 . ?
C57 C58 1.395(7) . ?
C57 H57 0.9500 . ?
C58 C59 1.369(8) . ?
C58 H58 0.9500 . ?
C59 C60 1.392(7) . ?
C59 H59 0.9500 . ?
C60 H60 0.9500 . ?

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 Al1 Cl1 180.00(5) . 2_766 ?
Cl1 Al1 P1 87.80(5) . . ?
Cl1 Al1 P1 92.20(5) 2_766 . ?
Cl1 Al1 P1 92.20(5) . 2_766 ?
Cl1 Al1 P1 87.80(5) 2_766 2_766 ?
P1 Al1 P1 180.00(5) . 2_766 ?
Cl1 Al1 P2 87.13(5) . . ?
Cl1 Al1 P2 92.87(5) 2_766 . ?
P1 Al1 P2 78.69(4) . . ?
P1 Al1 P2 101.31(4) 2_766 . ?
Cl1 Al1 P2 92.87(5) . 2_766 ?
Cl1 Al1 P2 87.13(5) 2_766 2_766 ?
P1 Al1 P2 101.31(4) . 2_766 ?
P1 Al1 P2 78.69(4) 2_766 2_766 ?
P2 Al1 P2 180.000(1) . 2_766 ?
Cl2 Al2 Cl2 180.00(6) . 2_565 ?
Cl2 Al2 P3 91.25(5) . 2_565 ?
Cl2 Al2 P3 88.75(5) 2_565 2_565 ?
Cl2 Al2 P3 88.75(5) . . ?
Cl2 Al2 P3 91.25(5) 2_565 . ?
P3 Al2 P3 180.0 2_565 . ?
Cl2 Al2 P4 94.66(5) . 2_565 ?
Cl2 Al2 P4 85.34(5) 2_565 2_565 ?
P3 Al2 P4 77.46(4) 2_565 2_565 ?
P3 Al2 P4 102.54(4) . 2_565 ?
Cl2 Al2 P4 85.34(5) . . ?
Cl2 Al2 P4 94.66(5) 2_565 . ?
P3 Al2 P4 102.54(4) 2_565 . ?
P3 Al2 P4 77.46(4) . . ?
P4 Al2 P4 180.0 2_565 . ?
Cl4 Al3 Cl6 109.42(9) . . ?
Cl4 Al3 Cl3 109.70(10) . . ?
Cl6 Al3 Cl3 108.49(9) . . ?
Cl4 Al3 Cl5 110.61(10) . . ?
Cl6 Al3 Cl5 110.25(9) . . ?
Cl3 Al3 Cl5 108.33(9) . . ?
C1 P1 C13 104.8(2) . . ?
C1 P1 C7 107.5(2) . . ?
C13 P1 C7 103.6(2) . . ?
C1 P1 Al1 116.34(15) . . ?
C13 P1 Al1 107.20(16) . . ?
C7 P1 Al1 116.01(16) . . ?
C18 P2 C19 103.9(2) . . ?
C18 P2 C25 103.2(2) . . ?
C19 P2 C25 107.2(2) . . ?
C18 P2 Al1 106.21(15) . . ?
C19 P2 Al1 117.56(15) . . ?
C25 P2 Al1 117.03(15) . . ?
C37 P3 C43 104.8(2) . . ?
C37 P3 C31 105.6(2) . . ?
C43 P3 C31 104.4(2) . . ?
C37 P3 Al2 115.41(17) . . ?
C43 P3 Al2 104.35(16) . . ?
C31 P3 Al2 120.68(18) . . ?
C48 P4 C49 103.6(2) . . ?
C48 P4 C55 106.2(2) . . ?
C49 P4 C55 104.4(2) . . ?
C48 P4 Al2 104.19(17) . . ?
C49 P4 Al2 121.92(18) . . ?
C55 P4 Al2 114.98(17) . . ?
C6 C1 C2 118.6(4) . . ?
C6 C1 P1 122.8(4) . . ?
C2 C1 P1 118.2(4) . . ?
C3 C2 C1 120.6(5) . . ?
C3 C2 H2 119.7 . . ?
C1 C2 H2 119.7 . . ?
C2 C3 C4 120.0(5) . . ?
C2 C3 H3 120.0 . . ?
C4 C3 H3 120.0 . . ?
C5 C4 C3 119.6(5) . . ?
C5 C4 H4 120.2 . . ?
C3 C4 H4 120.2 . . ?
C6 C5 C4 120.3(5) . . ?
C6 C5 H5 119.9 . . ?
C4 C5 H5 119.9 . . ?
C5 C6 C1 120.8(5) . . ?
C5 C6 H6 119.6 . . ?
C1 C6 H6 119.6 . . ?
C12 C7 C8 120.1(5) . . ?
C12 C7 P1 118.2(4) . . ?
C8 C7 P1 121.3(4) . . ?
C9 C8 C7 119.2(5) . . ?
C9 C8 H8 120.4 . . ?
C7 C8 H8 120.4 . . ?
C10 C9 C8 120.6(5) . . ?
C10 C9 H9 119.7 . . ?
C8 C9 H9 119.7 . . ?
C9 C10 C11 120.9(5) . . ?
C9 C10 H10 119.6 . . ?
C11 C10 H10 119.6 . . ?
C10 C11 C12 118.6(5) . . ?
C10 C11 H11 120.7 . . ?
C12 C11 H11 120.7 . . ?
C7 C12 C11 120.5(5) . . ?
C7 C12 H12 119.8 . . ?
C11 C12 H12 119.8 . . ?
C14 C13 C18 119.9(4) . . ?
C14 C13 P1 120.3(4) . . ?
C18 C13 P1 119.7(4) . . ?
C15 C14 C13 121.6(4) . . ?
C15 C14 H14 119.2 . . ?
C13 C14 H14 119.2 . . ?
C14 C15 C16 118.7(4) . . ?
C14 C15 H15 120.6 . . ?
C16 C15 H15 120.6 . . ?
C17 C16 C15 120.4(4) . . ?
C17 C16 H16 119.8 . . ?
C15 C16 H16 119.8 . . ?
C16 C17 C18 120.8(4) . . ?
C16 C17 H17 119.6 . . ?
C18 C17 H17 119.6 . . ?
C17 C18 C13 118.6(4) . . ?
C17 C18 P2 120.0(3) . . ?
C13 C18 P2 121.3(3) . . ?
C24 C19 C20 119.1(5) . . ?
C24 C19 P2 122.7(4) . . ?
C20 C19 P2 118.1(4) . . ?
C21 C20 C19 120.6(5) . . ?
C21 C20 H20 119.7 . . ?
C19 C20 H20 119.7 . . ?
C22 C21 C20 119.5(5) . . ?
C22 C21 H21 120.2 . . ?
C20 C21 H21 120.2 . . ?
C21 C22 C23 120.7(5) . . ?
C21 C22 H22 119.7 . . ?
C23 C22 H22 119.7 . . ?
C24 C23 C22 119.7(5) . . ?
C24 C23 H23 120.2 . . ?
C22 C23 H23 120.2 . . ?
C23 C24 C19 120.4(5) . . ?
C23 C24 H24 119.8 . . ?
C19 C24 H24 119.8 . . ?
C30 C25 C26 119.5(4) . . ?
C30 C25 P2 121.4(4) . . ?
C26 C25 P2 118.8(4) . . ?
C27 C26 C25 119.8(5) . . ?
C27 C26 H26 120.1 . . ?
C25 C26 H26 120.1 . . ?
C26 C27 C28 120.5(5) . . ?
C26 C27 H27 119.8 . . ?
C28 C27 H27 119.8 . . ?
C29 C28 C27 119.8(5) . . ?
C29 C28 H28 120.1 . . ?
C27 C28 H28 120.1 . . ?
C28 C29 C30 120.6(5) . . ?
C28 C29 H29 119.7 . . ?
C30 C29 H29 119.7 . . ?
C29 C30 C25 119.9(5) . . ?
C29 C30 H30 120.1 . . ?
C25 C30 H30 120.1 . . ?
C32 C31 C36 118.9(5) . . ?
C32 C31 P3 122.3(4) . . ?
C36 C31 P3 118.7(4) . . ?
C31 C32 C33 120.4(5) . . ?
C31 C32 H32 119.8 . . ?
C33 C32 H32 119.8 . . ?
C34 C33 C32 120.1(5) . . ?
C34 C33 H33 120.0 . . ?
C32 C33 H33 120.0 . . ?
C33 C34 C35 120.1(5) . . ?
C33 C34 H34 120.0 . . ?
C35 C34 H34 120.0 . . ?
C36 C35 C34 119.8(6) . . ?
C36 C35 H35 120.1 . . ?
C34 C35 H35 120.1 . . ?
C35 C36 C31 120.6(5) . . ?
C35 C36 H36 119.7 . . ?
C31 C36 H36 119.7 . . ?
C42 C37 C38 119.1(5) . . ?
C42 C37 P3 119.2(4) . . ?
C38 C37 P3 121.6(4) . . ?
C37 C38 C39 119.7(5) . . ?
C37 C38 H38 120.1 . . ?
C39 C38 H38 120.1 . . ?
C40 C39 C38 120.2(6) . . ?
C40 C39 H39 119.9 . . ?
C38 C39 H39 119.9 . . ?
C39 C40 C41 120.6(5) . . ?
C39 C40 H40 119.7 . . ?
C41 C40 H40 119.7 . . ?
C40 C41 C42 119.6(5) . . ?
C40 C41 H41 120.2 . . ?
C42 C41 H41 120.2 . . ?
C37 C42 C41 120.6(5) . . ?
C37 C42 H42 119.7 . . ?
C41 C42 H42 119.7 . . ?
C44 C43 C48 119.6(5) . . ?
C44 C43 P3 120.2(4) . . ?
C48 C43 P3 120.2(4) . . ?
C45 C44 C43 119.7(5) . . ?
C45 C44 H44 120.2 . . ?
C43 C44 H44 120.2 . . ?
C44 C45 C46 121.1(5) . . ?
C44 C45 H45 119.5 . . ?
C46 C45 H45 119.5 . . ?
C47 C46 C45 119.1(5) . . ?
C47 C46 H46 120.5 . . ?
C45 C46 H46 120.5 . . ?
C46 C47 C48 122.1(5) . . ?
C46 C47 H47 119.0 . . ?
C48 C47 H47 119.0 . . ?
C47 C48 C43 118.4(5) . . ?
C47 C48 P4 123.1(4) . . ?
C43 C48 P4 118.5(4) . . ?
C54 C49 C50 119.9(5) . . ?
C54 C49 P4 117.8(4) . . ?
C50 C49 P4 122.2(4) . . ?
C51 C50 C49 119.9(6) . . ?
C51 C50 H50 120.1 . . ?
C49 C50 H50 120.1 . . ?
C50 C51 C52 120.2(6) . . ?
C50 C51 H51 119.9 . . ?
C52 C51 H51 119.9 . . ?
C53 C52 C51 120.2(6) . . ?
C53 C52 H52 119.9 . . ?
C51 C52 H52 119.9 . . ?
C52 C53 C54 119.7(6) . . ?
C52 C53 H53 120.2 . . ?
C54 C53 H53 120.2 . . ?
C49 C54 C53 120.1(6) . . ?
C49 C54 H54 119.9 . . ?
C53 C54 H54 119.9 . . ?
C56 C55 C60 118.8(5) . . ?
C56 C55 P4 121.5(4) . . ?
C60 C55 P4 119.4(4) . . ?
C57 C56 C55 120.6(5) . . ?
C57 C56 H56 119.7 . . ?
C55 C56 H56 119.7 . . ?
C56 C57 C58 119.9(5) . . ?
C56 C57 H57 120.0 . . ?
C58 C57 H57 120.0 . . ?
C59 C58 C57 120.0(5) . . ?
C59 C58 H58 120.0 . . ?
C57 C58 H58 120.0 . . ?
C58 C59 C60 120.7(5) . . ?
C58 C59 H59 119.7 . . ?
C60 C59 H59 119.7 . . ?
C59 C60 C55 119.9(5) . . ?
C59 C60 H60 120.0 . . ?
C55 C60 H60 120.0 . . ?

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
C13 P1 C1 C6 4.4(4) . . . . ?
C7 P1 C1 C6 114.2(4) . . . . ?
Al1 P1 C1 C6 -113.8(4) . . . . ?
C13 P1 C1 C2 177.7(4) . . . . ?
C7 P1 C1 C2 -72.5(4) . . . . ?
Al1 P1 C1 C2 59.5(4) . . . . ?
C6 C1 C2 C3 -4.2(7) . . . . ?
P1 C1 C2 C3 -177.8(4) . . . . ?
C1 C2 C3 C4 3.0(7) . . . . ?
C2 C3 C4 C5 -0.7(7) . . . . ?
C3 C4 C5 C6 -0.4(7) . . . . ?
C4 C5 C6 C1 -0.8(7) . . . . ?
C2 C1 C6 C5 3.0(7) . . . . ?
P1 C1 C6 C5 176.4(4) . . . . ?
C1 P1 C7 C12 -157.3(4) . . . . ?
C13 P1 C7 C12 -46.6(4) . . . . ?
Al1 P1 C7 C12 70.5(4) . . . . ?
C1 P1 C7 C8 30.1(5) . . . . ?
C13 P1 C7 C8 140.7(4) . . . . ?
Al1 P1 C7 C8 -102.1(4) . . . . ?
C12 C7 C8 C9 -3.2(7) . . . . ?
P1 C7 C8 C9 169.3(4) . . . . ?
C7 C8 C9 C10 0.8(7) . . . . ?
C8 C9 C10 C11 3.3(8) . . . . ?
C9 C10 C11 C12 -4.9(8) . . . . ?
C8 C7 C12 C11 1.6(7) . . . . ?
P1 C7 C12 C11 -171.2(4) . . . . ?
C10 C11 C12 C7 2.4(7) . . . . ?
C1 P1 C13 C14 71.5(4) . . . . ?
C7 P1 C13 C14 -41.1(4) . . . . ?
Al1 P1 C13 C14 -164.3(4) . . . . ?
C1 P1 C13 C18 -105.3(4) . . . . ?
C7 P1 C13 C18 142.1(4) . . . . ?
Al1 P1 C13 C18 18.9(4) . . . . ?
C18 C13 C14 C15 0.3(7) . . . . ?
P1 C13 C14 C15 -176.5(4) . . . . ?
C13 C14 C15 C16 -0.5(7) . . . . ?
C14 C15 C16 C17 0.0(7) . . . . ?
C15 C16 C17 C18 0.8(7) . . . . ?
C16 C17 C18 C13 -1.0(7) . . . . ?
C16 C17 C18 P2 175.8(4) . . . . ?
C14 C13 C18 C17 0.5(7) . . . . ?
P1 C13 C18 C17 177.3(4) . . . . ?
C14 C13 C18 P2 -176.3(4) . . . . ?
P1 C13 C18 P2 0.6(6) . . . . ?
C19 P2 C18 C17 -71.5(4) . . . . ?
C25 P2 C18 C17 40.2(4) . . . . ?
Al1 P2 C18 C17 163.9(3) . . . . ?
C19 P2 C18 C13 105.2(4) . . . . ?
C25 P2 C18 C13 -143.1(4) . . . . ?
Al1 P2 C18 C13 -19.4(4) . . . . ?
C18 P2 C19 C24 2.4(5) . . . . ?
C25 P2 C19 C24 -106.4(4) . . . . ?
Al1 P2 C19 C24 119.3(4) . . . . ?
C18 P2 C19 C20 -174.6(4) . . . . ?
C25 P2 C19 C20 76.6(4) . . . . ?
Al1 P2 C19 C20 -57.6(4) . . . . ?
C24 C19 C20 C21 1.9(7) . . . . ?
P2 C19 C20 C21 179.0(4) . . . . ?
C19 C20 C21 C22 -0.7(8) . . . . ?
C20 C21 C22 C23 -0.9(8) . . . . ?
C21 C22 C23 C24 1.2(8) . . . . ?
C22 C23 C24 C19 0.1(8) . . . . ?
C20 C19 C24 C23 -1.6(7) . . . . ?
P2 C19 C24 C23 -178.5(4) . . . . ?
C18 P2 C25 C30 -142.9(4) . . . . ?
C19 P2 C25 C30 -33.6(4) . . . . ?
Al1 P2 C25 C30 101.0(4) . . . . ?
C18 P2 C25 C26 44.1(4) . . . . ?
C19 P2 C25 C26 153.4(4) . . . . ?
Al1 P2 C25 C26 -72.1(4) . . . . ?
C30 C25 C26 C27 1.2(7) . . . . ?
P2 C25 C26 C27 174.4(4) . . . . ?
C25 C26 C27 C28 -1.6(8) . . . . ?
C26 C27 C28 C29 1.4(8) . . . . ?
C27 C28 C29 C30 -0.8(8) . . . . ?
C28 C29 C30 C25 0.4(8) . . . . ?
C26 C25 C30 C29 -0.6(7) . . . . ?
P2 C25 C30 C29 -173.6(4) . . . . ?
C37 P3 C31 C32 -4.7(5) . . . . ?
C43 P3 C31 C32 -114.8(5) . . . . ?
Al2 P3 C31 C32 128.4(4) . . . . ?
C37 P3 C31 C36 177.5(4) . . . . ?
C43 P3 C31 C36 67.4(5) . . . . ?
Al2 P3 C31 C36 -49.4(5) . . . . ?
C36 C31 C32 C33 2.7(9) . . . . ?
P3 C31 C32 C33 -175.1(4) . . . . ?
C31 C32 C33 C34 0.4(9) . . . . ?
C32 C33 C34 C35 -3.0(9) . . . . ?
C33 C34 C35 C36 2.4(10) . . . . ?
C34 C35 C36 C31 0.7(9) . . . . ?
C32 C31 C36 C35 -3.3(9) . . . . ?
P3 C31 C36 C35 174.6(5) . . . . ?
C43 P3 C37 C42 175.3(4) . . . . ?
C31 P3 C37 C42 65.4(4) . . . . ?
Al2 P3 C37 C42 -70.5(4) . . . . ?
C43 P3 C37 C38 -5.1(5) . . . . ?
C31 P3 C37 C38 -115.0(4) . . . . ?
Al2 P3 C37 C38 109.1(4) . . . . ?
C42 C37 C38 C39 1.2(7) . . . . ?
P3 C37 C38 C39 -178.4(4) . . . . ?
C37 C38 C39 C40 -3.8(8) . . . . ?
C38 C39 C40 C41 2.9(8) . . . . ?
C39 C40 C41 C42 0.8(8) . . . . ?
C38 C37 C42 C41 2.4(7) . . . . ?
P3 C37 C42 C41 -177.9(4) . . . . ?
C40 C41 C42 C37 -3.4(8) . . . . ?
C37 P3 C43 C44 -83.3(5) . . . . ?
C31 P3 C43 C44 27.5(5) . . . . ?
Al2 P3 C43 C44 155.0(4) . . . . ?
C37 P3 C43 C48 97.3(5) . . . . ?
C31 P3 C43 C48 -152.0(4) . . . . ?
Al2 P3 C43 C48 -24.4(5) . . . . ?
C48 C43 C44 C45 0.7(8) . . . . ?
P3 C43 C44 C45 -178.8(4) . . . . ?
C43 C44 C45 C46 1.8(9) . . . . ?
C44 C45 C46 C47 -2.8(9) . . . . ?
C45 C46 C47 C48 1.4(9) . . . . ?
C46 C47 C48 C43 1.0(8) . . . . ?
C46 C47 C48 P4 -176.9(4) . . . . ?
C44 C43 C48 C47 -2.0(8) . . . . ?
P3 C43 C48 C47 177.4(4) . . . . ?
C44 C43 C48 P4 175.9(4) . . . . ?
P3 C43 C48 P4 -4.6(6) . . . . ?
C49 P4 C48 C47 80.5(5) . . . . ?
C55 P4 C48 C47 -29.2(5) . . . . ?
Al2 P4 C48 C47 -151.0(4) . . . . ?
C49 P4 C48 C43 -97.3(5) . . . . ?
C55 P4 C48 C43 153.0(4) . . . . ?
Al2 P4 C48 C43 31.2(4) . . . . ?
C48 P4 C49 C54 167.1(4) . . . . ?
C55 P4 C49 C54 -81.9(5) . . . . ?
Al2 P4 C49 C54 50.5(5) . . . . ?
C48 P4 C49 C50 -14.4(5) . . . . ?
C55 P4 C49 C50 96.6(5) . . . . ?
Al2 P4 C49 C50 -131.0(4) . . . . ?
C54 C49 C50 C51 2.5(8) . . . . ?
P4 C49 C50 C51 -176.0(4) . . . . ?
C49 C50 C51 C52 -0.8(9) . . . . ?
C50 C51 C52 C53 -0.5(10) . . . . ?
C51 C52 C53 C54 0.0(10) . . . . ?
C50 C49 C54 C53 -3.1(8) . . . . ?
P4 C49 C54 C53 175.5(5) . . . . ?
C52 C53 C54 C49 1.8(9) . . . . ?
C48 P4 C55 C56 -38.7(5) . . . . ?
C49 P4 C55 C56 -147.8(4) . . . . ?
Al2 P4 C55 C56 75.9(5) . . . . ?
C48 P4 C55 C60 147.2(4) . . . . ?
C49 P4 C55 C60 38.1(5) . . . . ?
Al2 P4 C55 C60 -98.2(4) . . . . ?
C60 C55 C56 C57 -2.8(8) . . . . ?
P4 C55 C56 C57 -177.0(4) . . . . ?
C55 C56 C57 C58 0.7(8) . . . . ?
C56 C57 C58 C59 2.3(8) . . . . ?
C57 C58 C59 C60 -3.0(9) . . . . ?
C58 C59 C60 C55 0.8(8) . . . . ?
C56 C55 C60 C59 2.1(8) . . . . ?
P4 C55 C60 C59 176.4(4) . . . . ?

_diffrn_measured_fraction_theta_max 0.943
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.943
_refine_diff_density_max         0.554
_refine_diff_density_min         -0.484
_refine_diff_density_rms         0.095

_iucr_refine_instruction_details 
;
 Add final .res file here for Acta Cryst publications or if required.
;
_database_code_depnum_ccdc_archive 'CCDC 1005863'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_[(AlCl3)2{?-Me2P(CH2)2PMe2}]
#data_13jebr17 

_audit_creation_method           'SHELXL-97 + hand edit'
_audit_creation_date             2013-08-19 # yyyy-mm-dd

_chemical_name_systematic        
; 
  1,2-Bis(dimethylphosphino)ethane-bis(trichloroaluminium(III))
;

# Me2PCH2CH2PMe2 = C6H16P2 = dmpe
# ethane-1,2-diylbis(dimethylphosphine)  (iLab defaults)
# ethane-1,2-diylbis(dimethylphosphane)  (iLab selected options)
# 2-dimethylphosphanylethyl-dimethyl-phosphane  (chemspider)
# 1,2-Bis(dimethylphosphino)ethane (chemspider alternative) 
# [2-(Dimethylphosphino)ethyl](dimethyl)phosphine (chemspider)

_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C6 H16 Al2 Cl6 P2'
_chemical_formula_sum            'C6 H16 Al2 Cl6 P2'
_chemical_formula_weight         416.79

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'
Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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_name_H-M_alt        'P 21/c'
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'


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

_cell_length_a                   10.738(6)
_cell_length_b                   7.948(4)
_cell_length_c                   11.772(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 113.938(9)
_cell_angle_gamma                90.00
_cell_volume                     918.2(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    3083
_cell_measurement_theta_min      3.2
_cell_measurement_theta_max      34.7

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.507
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             420
_exptl_absorpt_coefficient_mu    1.182
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.812 # Expt'l Tmin & Tmax 
_exptl_absorpt_correction_T_max  1.000 # scaled to Tmax=1.0 
_exptl_absorpt_process_details   
;Jacobson, R.A. (1998). REQAB. Private communication to the 
 Rigaku Corporation, Tokyo, Japan. 
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  ?
_diffrn_radiation_collimation    'Confocal mirrors, VHF VariMax '

_diffrn_source                   'Rotating anode X-ray tube'
_diffrn_source_type              'Rigaku FR-E+ Superbright'

_diffrn_measurement_device       'Four-circle κ diffractometer'
_diffrn_measurement_device_type  'Rigaku AFC12 '
_diffrn_measurement_method       'Profile data from ω-scans'

_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Rigaku HG Saturn724+ (2x2 bin mode)'
_diffrn_detector_area_resol_mean ?

_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            10169
_diffrn_reflns_av_R_equivalents  0.0624
# _diffrn_reflns_av_sigmaI/netI   0.0588
_diffrn_reflns_av_unetI/netI     0.0588
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         3.19
_diffrn_reflns_theta_max         27.49
_reflns_number_total             2093
_reflns_number_gt                1787
_reflns_threshold_expression     I>2σ(I)

_computing_data_collection       'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)'
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'ORTEP-III (Farrugia, 1997)'
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0169P)²+0.4336P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2093
_refine_ls_number_parameters     73
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0647
_refine_ls_R_factor_gt           0.0506
_refine_ls_wR_factor_ref         0.0805
_refine_ls_wR_factor_gt          0.0764
_refine_ls_goodness_of_fit_ref   1.182
_refine_ls_restrained_S_all      1.182
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Al1 Al 0.25873(9) 0.33799(12) -0.09842(8) 0.0199(2) Uani 1 1 d . . .
Cl1 Cl 0.09922(8) 0.15904(10) -0.13723(7) 0.0285(2) Uani 1 1 d . . .
Cl2 Cl 0.45314(8) 0.23518(12) 0.00873(7) 0.0355(2) Uani 1 1 d . . .
Cl3 Cl 0.25002(8) 0.45108(11) -0.26461(7) 0.0295(2) Uani 1 1 d . . .
P1 P 0.21668(8) 0.54576(10) 0.03047(7) 0.01805(19) Uani 1 1 d . . .
C1 C 0.3533(3) 0.5585(4) 0.1835(3) 0.0283(8) Uani 1 1 d . . .
H1A H 0.3722 0.4461 0.2209 0.042 Uiso 1 1 calc R . .
H1B H 0.3266 0.6336 0.2357 0.042 Uiso 1 1 calc R . .
H1C H 0.4353 0.6025 0.1768 0.042 Uiso 1 1 calc R . .
C2 C 0.1882(3) 0.7563(4) -0.0324(3) 0.0256(7) Uani 1 1 d . . .
H2A H 0.1146 0.7548 -0.1159 0.038 Uiso 1 1 calc R . .
H2B H 0.2718 0.7986 -0.0370 0.038 Uiso 1 1 calc R . .
H2C H 0.1627 0.8300 0.0215 0.038 Uiso 1 1 calc R . .
C3 C 0.0678(3) 0.4904(4) 0.0581(2) 0.0193(7) Uani 1 1 d . . .
H3A H 0.0767 0.3723 0.0871 0.023 Uiso 1 1 calc R . .
H3B H 0.0644 0.5626 0.1253 0.023 Uiso 1 1 calc R . .


_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
Al1 Cl2 2.1166(14) . ?
Al1 Cl3 2.1203(15) . ?
Al1 Cl1 2.1284(15) . ?
Al1 P1 2.4059(14) . ?
P1 C2 1.805(3) . ?
P1 C3 1.811(3) . ?
P1 C1 1.806(3) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 C3 1.548(5) 3_565 ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?

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 Al1 Cl3 112.15(6) . . ?
Cl2 Al1 Cl1 112.54(6) . . ?
Cl3 Al1 Cl1 110.78(5) . . ?
Cl2 Al1 P1 106.34(5) . . ?
Cl3 Al1 P1 109.97(6) . . ?
Cl1 Al1 P1 104.68(5) . . ?
C2 P1 C3 106.51(14) . . ?
C2 P1 C1 106.92(15) . . ?
C3 P1 C1 104.70(14) . . ?
C2 P1 Al1 114.94(11) . . ?
C3 P1 Al1 110.60(11) . . ?
C1 P1 Al1 112.50(11) . . ?
P1 C1 H1A 109.5 . . ?
P1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
P1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
P1 C2 H2A 109.5 . . ?
P1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
P1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C3 C3 P1 113.5(3) 3_565 . ?
C3 C3 H3A 108.9 3_565 . ?
P1 C3 H3A 108.9 . . ?
C3 C3 H3B 108.9 3_565 . ?
P1 C3 H3B 108.9 . . ?
H3A C3 H3B 107.7 . . ?

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
Cl2 Al1 P1 C2 120.81(12) . . . . ?
Cl3 Al1 P1 C2 -0.83(12) . . . . ?
Cl1 Al1 P1 C2 -119.88(12) . . . . ?
Cl2 Al1 P1 C3 -118.56(11) . . . . ?
Cl3 Al1 P1 C3 119.80(11) . . . . ?
Cl1 Al1 P1 C3 0.75(11) . . . . ?
Cl2 Al1 P1 C1 -1.88(13) . . . . ?
Cl3 Al1 P1 C1 -123.52(13) . . . . ?
Cl1 Al1 P1 C1 117.44(13) . . . . ?
C2 P1 C3 C3 54.6(3) . . . 3_565 ?
C1 P1 C3 C3 167.6(3) . . . 3_565 ?
Al1 P1 C3 C3 -70.9(3) . . . 3_565 ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        27.49
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.383
_refine_diff_density_min         -0.287
_refine_diff_density_rms         0.080

_iucr_refine_instruction_details 
;
 Add final .res file here for Acta Cryst publications or if required.
;
_database_code_depnum_ccdc_archive 'CCDC 1005864'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_[AlCl2{Me2P(CH2)2Me2}2][AlCl4]
#data_13jebr26_ml

_audit_creation_method           'SHELXL-97 + hand edit'
_chemical_name_systematic        
;
  dichlorobis(ethane-1,2-diylbis(dimethylphosphine))aluminium 
 tetrachloroaluminate 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H32 Al Cl2 P4 1+, Al Cl4 1-'
_chemical_formula_sum            'C12 H32 Al2 Cl6 P4'
_chemical_formula_weight         566.92

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'
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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

loop_
_symmetry_equiv_pos_as_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                   19.631(5)
_cell_length_b                   16.157(4)
_cell_length_c                   34.831(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     11048(5)
_cell_formula_units_Z            16
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    22170
_cell_measurement_theta_min      1.7
_cell_measurement_theta_max      27.5

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.363
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4672
_exptl_absorpt_coefficient_mu    0.916
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9471
_exptl_absorpt_correction_T_max  0.9556
_exptl_absorpt_process_details   'CrystalClear-SM Expert 2.0 r11 (Rigaku, 2011)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source_power             2.5
_diffrn_source_voltage           45.0
_diffrn_source_current           55.0
_diffrn_source                   'Rotating Anode'
_diffrn_radiation_monochromator  Confocal
_diffrn_measurement_specimen_support Mitegen
_diffrn_detector                 CCD
_diffrn_measurement_device       
;
AFC12 (Right): Kappa 3 circle
;
_diffrn_measurement_device_type  
;
Rigaku Saturn724+ (2x2 bin mode)
;
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            92232
_diffrn_reflns_av_R_equivalents  0.1169
_diffrn_reflns_av_sigmaI/netI    0.0592
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_theta_min         1.73
_diffrn_reflns_theta_max         26.00
_reflns_number_total             10858
_reflns_number_gt                7635
_reflns_threshold_expression     >2σ(I)

_computing_data_collection       
;
CrystalClear-SM Expert 2.0 r11 (Rigaku, 2011)
;
_computing_cell_refinement       
;
CrystalClear-SM Expert 2.0 r11 (Rigaku, 2011)
;
_computing_data_reduction        
;
CrystalClear-SM Expert 2.0 r11 (Rigaku, 2011)
;
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0333P)²+25.5662P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         10858
_refine_ls_number_parameters     449
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0871
_refine_ls_R_factor_gt           0.0503
_refine_ls_wR_factor_ref         0.1148
_refine_ls_wR_factor_gt          0.0985
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_restrained_S_all      1.051
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cl1 Cl 0.45650(5) 0.23812(6) 0.17785(3) 0.0238(2) Uani 1 1 d . . .
Cl2 Cl 0.55265(5) 0.23547(6) 0.05783(3) 0.0224(2) Uani 1 1 d . . .
P1 P 0.41275(6) 0.14169(6) 0.09565(3) 0.0213(2) Uani 1 1 d . . .
P2 P 0.42625(5) 0.34588(6) 0.09469(3) 0.0190(2) Uani 1 1 d . . .
P3 P 0.59420(6) 0.33280(6) 0.14163(3) 0.0193(2) Uani 1 1 d . . .
P4 P 0.58735(6) 0.12792(6) 0.13776(3) 0.0201(2) Uani 1 1 d . . .
Al1 Al 0.50466(6) 0.23669(7) 0.11794(3) 0.0175(3) Uani 1 1 d . . .
C1 C 0.4288(2) 0.0826(3) 0.05208(14) 0.0362(12) Uani 1 1 d . . .
H1A H 0.4647 0.0417 0.0570 0.054 Uiso 1 1 calc R . .
H1B H 0.4433 0.1201 0.0316 0.054 Uiso 1 1 calc R . .
H1C H 0.3870 0.0540 0.0443 0.054 Uiso 1 1 calc R . .
C2 C 0.3769(2) 0.0677(3) 0.12955(14) 0.0328(11) Uani 1 1 d . . .
H2A H 0.3674 0.0957 0.1539 0.049 Uiso 1 1 calc R . .
H2B H 0.4095 0.0228 0.1339 0.049 Uiso 1 1 calc R . .
H2C H 0.3345 0.0449 0.1191 0.049 Uiso 1 1 calc R . .
C3 C 0.3411(2) 0.2102(3) 0.08323(13) 0.0264(10) Uani 1 1 d . . .
H3A H 0.3096 0.1806 0.0658 0.032 Uiso 1 1 calc R . .
H3B H 0.3157 0.2246 0.1069 0.032 Uiso 1 1 calc R . .
C4 C 0.3659(2) 0.2900(3) 0.06362(12) 0.0251(10) Uani 1 1 d . . .
H4A H 0.3264 0.3261 0.0579 0.030 Uiso 1 1 calc R . .
H4B H 0.3884 0.2761 0.0390 0.030 Uiso 1 1 calc R . .
C5 C 0.3743(2) 0.3990(3) 0.13016(12) 0.0259(10) Uani 1 1 d . . .
H5A H 0.4037 0.4319 0.1471 0.039 Uiso 1 1 calc R . .
H5B H 0.3492 0.3582 0.1455 0.039 Uiso 1 1 calc R . .
H5C H 0.3420 0.4357 0.1171 0.039 Uiso 1 1 calc R . .
C6 C 0.4616(2) 0.4274(2) 0.06495(12) 0.0251(10) Uani 1 1 d . . .
H6A H 0.4245 0.4587 0.0530 0.038 Uiso 1 1 calc R . .
H6B H 0.4903 0.4028 0.0449 0.038 Uiso 1 1 calc R . .
H6C H 0.4892 0.4645 0.0809 0.038 Uiso 1 1 calc R . .
C7 C 0.5687(2) 0.4149(3) 0.17416(13) 0.0282(10) Uani 1 1 d . . .
H7A H 0.6090 0.4373 0.1871 0.042 Uiso 1 1 calc R . .
H7B H 0.5371 0.3927 0.1934 0.042 Uiso 1 1 calc R . .
H7C H 0.5462 0.4590 0.1596 0.042 Uiso 1 1 calc R . .
C8 C 0.6478(2) 0.3831(3) 0.10604(12) 0.0284(10) Uani 1 1 d . . .
H8A H 0.6202 0.4210 0.0906 0.043 Uiso 1 1 calc R . .
H8B H 0.6683 0.3411 0.0893 0.043 Uiso 1 1 calc R . .
H8C H 0.6839 0.4142 0.1190 0.043 Uiso 1 1 calc R . .
C9 C 0.6522(2) 0.2661(2) 0.16879(12) 0.0219(9) Uani 1 1 d . . .
H9A H 0.6956 0.2958 0.1734 0.026 Uiso 1 1 calc R . .
H9B H 0.6317 0.2526 0.1940 0.026 Uiso 1 1 calc R . .
C10 C 0.6665(2) 0.1855(3) 0.14645(13) 0.0240(9) Uani 1 1 d . . .
H10A H 0.6984 0.1505 0.1613 0.029 Uiso 1 1 calc R . .
H10B H 0.6883 0.1990 0.1216 0.029 Uiso 1 1 calc R . .
C11 C 0.6124(2) 0.0489(3) 0.10348(13) 0.0271(10) Uani 1 1 d . . .
H11A H 0.6530 0.0201 0.1129 0.041 Uiso 1 1 calc R . .
H11B H 0.6225 0.0749 0.0787 0.041 Uiso 1 1 calc R . .
H11C H 0.5751 0.0092 0.1003 0.041 Uiso 1 1 calc R . .
C12 C 0.5702(2) 0.0726(3) 0.18226(12) 0.0276(10) Uani 1 1 d . . .
H12A H 0.5260 0.0448 0.1804 0.041 Uiso 1 1 calc R . .
H12B H 0.5694 0.1120 0.2037 0.041 Uiso 1 1 calc R . .
H12C H 0.6060 0.0315 0.1866 0.041 Uiso 1 1 calc R . .
Cl3 Cl 0.02627(6) 0.09822(6) 0.13012(3) 0.0259(2) Uani 1 1 d . . .
Cl4 Cl 0.00519(5) 0.37991(6) 0.13490(3) 0.0223(2) Uani 1 1 d . . .
P5 P -0.10172(6) 0.22563(7) 0.10461(3) 0.0212(2) Uani 1 1 d . . .
P6 P 0.04994(6) 0.24488(6) 0.06368(3) 0.0212(2) Uani 1 1 d . . .
P7 P 0.13226(6) 0.24687(7) 0.16084(3) 0.0221(2) Uani 1 1 d . . .
P8 P -0.02038(6) 0.23678(7) 0.20120(3) 0.0205(2) Uani 1 1 d . . .
Al2 Al 0.01520(6) 0.23876(7) 0.13270(3) 0.0179(3) Uani 1 1 d . . .
C13 C -0.1660(2) 0.3026(3) 0.11605(14) 0.0306(11) Uani 1 1 d . . .
H13A H -0.2052 0.2956 0.0990 0.046 Uiso 1 1 calc R . .
H13B H -0.1468 0.3581 0.1126 0.046 Uiso 1 1 calc R . .
H13C H -0.1806 0.2957 0.1428 0.046 Uiso 1 1 calc R . .
C14 C -0.1453(2) 0.1278(3) 0.11178(13) 0.0308(11) Uani 1 1 d . . .
H14A H -0.1549 0.1202 0.1392 0.046 Uiso 1 1 calc R . .
H14B H -0.1164 0.0824 0.1027 0.046 Uiso 1 1 calc R . .
H14C H -0.1882 0.1279 0.0974 0.046 Uiso 1 1 calc R . .
C15 C -0.0905(2) 0.2348(3) 0.05228(12) 0.0291(10) Uani 1 1 d . . .
H15A H -0.1284 0.2060 0.0392 0.035 Uiso 1 1 calc R . .
H15B H -0.0924 0.2940 0.0450 0.035 Uiso 1 1 calc R . .
C16 C -0.0224(2) 0.1979(3) 0.03867(12) 0.0316(11) Uani 1 1 d . . .
H16A H -0.0174 0.2069 0.0107 0.038 Uiso 1 1 calc R . .
H16B H -0.0224 0.1374 0.0434 0.038 Uiso 1 1 calc R . .
C17 C 0.0616(3) 0.3462(3) 0.04244(12) 0.0326(11) Uani 1 1 d . . .
H17A H 0.0700 0.3402 0.0148 0.049 Uiso 1 1 calc R . .
H17B H 0.1006 0.3737 0.0545 0.049 Uiso 1 1 calc R . .
H17C H 0.0205 0.3794 0.0465 0.049 Uiso 1 1 calc R . .
C18 C 0.1238(3) 0.1866(3) 0.04695(14) 0.0376(12) Uani 1 1 d . . .
H18A H 0.1247 0.1866 0.0188 0.056 Uiso 1 1 calc R . .
H18B H 0.1208 0.1295 0.0563 0.056 Uiso 1 1 calc R . .
H18C H 0.1655 0.2123 0.0568 0.056 Uiso 1 1 calc R . .
C19 C 0.1818(2) 0.3385(3) 0.15053(14) 0.0334(11) Uani 1 1 d . . .
H19A H 0.2225 0.3393 0.1668 0.050 Uiso 1 1 calc R . .
H19B H 0.1542 0.3879 0.1557 0.050 Uiso 1 1 calc R . .
H19C H 0.1955 0.3381 0.1235 0.050 Uiso 1 1 calc R . .
C20 C 0.1910(2) 0.1621(3) 0.15266(14) 0.0331(11) Uani 1 1 d . . .
H20A H 0.2030 0.1598 0.1254 0.050 Uiso 1 1 calc R . .
H20B H 0.1695 0.1099 0.1603 0.050 Uiso 1 1 calc R . .
H20C H 0.2323 0.1708 0.1679 0.050 Uiso 1 1 calc R . .
C21 C 0.1198(2) 0.2449(3) 0.21339(12) 0.0306(10) Uani 1 1 d . . .
H21A H 0.1217 0.1868 0.2224 0.037 Uiso 1 1 calc R . .
H21B H 0.1575 0.2754 0.2258 0.037 Uiso 1 1 calc R . .
C22 C 0.0521(2) 0.2830(3) 0.22595(13) 0.0323(11) Uani 1 1 d . . .
H22A H 0.0529 0.3432 0.2207 0.039 Uiso 1 1 calc R . .
H22B H 0.0465 0.2754 0.2540 0.039 Uiso 1 1 calc R . .
C23 C -0.0361(3) 0.1371(3) 0.22342(13) 0.0347(11) Uani 1 1 d . . .
H23A H 0.0035 0.1011 0.2195 0.052 Uiso 1 1 calc R . .
H23B H -0.0763 0.1116 0.2118 0.052 Uiso 1 1 calc R . .
H23C H -0.0438 0.1447 0.2510 0.052 Uiso 1 1 calc R . .
C24 C -0.0917(3) 0.3009(3) 0.21677(14) 0.0370(12) Uani 1 1 d . . .
H24A H -0.1344 0.2766 0.2077 0.056 Uiso 1 1 calc R . .
H24B H -0.0866 0.3567 0.2061 0.056 Uiso 1 1 calc R . .
H24C H -0.0922 0.3039 0.2449 0.056 Uiso 1 1 calc R . .
Cl5 Cl 0.70516(7) -0.07603(8) 0.02975(4) 0.0460(3) Uani 1 1 d . . .
Cl6 Cl 0.72812(7) 0.14035(8) 0.02164(4) 0.0439(3) Uani 1 1 d . . .
Cl7 Cl 0.86842(6) 0.00896(7) 0.01924(3) 0.0304(2) Uani 1 1 d . . .
Cl8 Cl 0.75391(6) 0.01032(8) -0.05744(3) 0.0393(3) Uani 1 1 d . . .
Al3 Al 0.76327(7) 0.02073(9) 0.00408(4) 0.0281(3) Uani 1 1 d . . .
Cl9 Cl 0.24207(6) -0.03252(8) 0.31422(3) 0.0371(3) Uani 1 1 d . . .
Cl10 Cl 0.16404(7) -0.00915(9) 0.22509(4) 0.0490(4) Uani 1 1 d . . .
Cl11 Cl 0.34370(7) -0.02520(9) 0.23174(4) 0.0475(3) Uani 1 1 d . . .
Cl12 Cl 0.26206(6) 0.15167(7) 0.26368(4) 0.0381(3) Uani 1 1 d . . .
Al4 Al 0.25273(7) 0.02000(8) 0.25776(4) 0.0289(3) Uani 1 1 d . . .


_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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 Al1 2.2911(16) . ?
Cl2 Al1 2.2959(16) . ?
P1 C1 1.820(4) . ?
P1 C2 1.821(4) . ?
P1 C3 1.841(4) . ?
P1 Al1 2.4929(16) . ?
P2 C6 1.814(4) . ?
P2 C5 1.818(4) . ?
P2 C4 1.841(4) . ?
P2 Al1 2.4773(16) . ?
P3 C7 1.815(4) . ?
P3 C8 1.818(4) . ?
P3 C9 1.831(4) . ?
P3 Al1 2.4863(16) . ?
P4 C11 1.815(4) . ?
P4 C12 1.820(4) . ?
P4 C10 1.836(4) . ?
P4 Al1 2.4899(16) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 C4 1.539(6) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 C10 1.543(6) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
Cl3 Al2 2.2828(16) . ?
Cl4 Al2 2.2903(16) . ?
P5 C14 1.815(4) . ?
P5 C13 1.815(4) . ?
P5 C15 1.842(4) . ?
P5 Al2 2.5042(17) . ?
P6 C17 1.811(4) . ?
P6 C18 1.824(5) . ?
P6 C16 1.830(5) . ?
P6 Al2 2.5011(16) . ?
P7 C19 1.808(5) . ?
P7 C20 1.813(4) . ?
P7 C21 1.847(4) . ?
P7 Al2 2.5017(17) . ?
P8 C23 1.814(4) . ?
P8 C22 1.823(5) . ?
P8 C24 1.824(5) . ?
P8 Al2 2.4860(16) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 C16 1.539(6) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 C22 1.529(6) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
Cl5 Al3 2.1318(18) . ?
Cl6 Al3 2.141(2) . ?
Cl7 Al3 2.1392(19) . ?
Cl8 Al3 2.1571(17) . ?
Cl9 Al4 2.1519(18) . ?
Cl10 Al4 2.1325(19) . ?
Cl11 Al4 2.132(2) . ?
Cl12 Al4 2.1453(19) . ?

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
C1 P1 C2 105.2(2) . . ?
C1 P1 C3 104.6(2) . . ?
C2 P1 C3 104.6(2) . . ?
C1 P1 Al1 117.23(16) . . ?
C2 P1 Al1 118.79(16) . . ?
C3 P1 Al1 104.82(14) . . ?
C6 P2 C5 105.1(2) . . ?
C6 P2 C4 105.4(2) . . ?
C5 P2 C4 105.7(2) . . ?
C6 P2 Al1 117.75(15) . . ?
C5 P2 Al1 117.58(15) . . ?
C4 P2 Al1 104.06(14) . . ?
C7 P3 C8 105.0(2) . . ?
C7 P3 C9 106.2(2) . . ?
C8 P3 C9 104.8(2) . . ?
C7 P3 Al1 117.93(16) . . ?
C8 P3 Al1 117.52(15) . . ?
C9 P3 Al1 104.10(14) . . ?
C11 P4 C12 105.4(2) . . ?
C11 P4 C10 103.6(2) . . ?
C12 P4 C10 105.3(2) . . ?
C11 P4 Al1 119.34(16) . . ?
C12 P4 Al1 117.51(15) . . ?
C10 P4 Al1 103.88(14) . . ?
Cl1 Al1 Cl2 179.83(8) . . ?
Cl1 Al1 P2 91.96(6) . . ?
Cl2 Al1 P2 87.88(5) . . ?
Cl1 Al1 P3 89.03(5) . . ?
Cl2 Al1 P3 91.02(5) . . ?
P2 Al1 P3 95.91(6) . . ?
Cl1 Al1 P4 91.35(5) . . ?
Cl2 Al1 P4 88.81(5) . . ?
P2 Al1 P4 176.64(6) . . ?
P3 Al1 P4 83.56(5) . . ?
Cl1 Al1 P1 89.50(5) . . ?
Cl2 Al1 P1 90.44(5) . . ?
P2 Al1 P1 83.51(5) . . ?
P3 Al1 P1 178.40(7) . . ?
P4 Al1 P1 97.10(6) . . ?
P1 C1 H1A 109.5 . . ?
P1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
P1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
P1 C2 H2A 109.5 . . ?
P1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
P1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C4 C3 P1 111.5(3) . . ?
C4 C3 H3A 109.3 . . ?
P1 C3 H3A 109.3 . . ?
C4 C3 H3B 109.3 . . ?
P1 C3 H3B 109.3 . . ?
H3A C3 H3B 108.0 . . ?
C3 C4 P2 110.7(3) . . ?
C3 C4 H4A 109.5 . . ?
P2 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
P2 C4 H4B 109.5 . . ?
H4A C4 H4B 108.1 . . ?
P2 C5 H5A 109.5 . . ?
P2 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
P2 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
P2 C6 H6A 109.5 . . ?
P2 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
P2 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
P3 C7 H7A 109.5 . . ?
P3 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
P3 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
P3 C8 H8A 109.5 . . ?
P3 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
P3 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C10 C9 P3 110.4(3) . . ?
C10 C9 H9A 109.6 . . ?
P3 C9 H9A 109.6 . . ?
C10 C9 H9B 109.6 . . ?
P3 C9 H9B 109.6 . . ?
H9A C9 H9B 108.1 . . ?
C9 C10 P4 110.9(3) . . ?
C9 C10 H10A 109.5 . . ?
P4 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
P4 C10 H10B 109.5 . . ?
H10A C10 H10B 108.0 . . ?
P4 C11 H11A 109.5 . . ?
P4 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
P4 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
P4 C12 H12A 109.5 . . ?
P4 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
P4 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C14 P5 C13 103.8(2) . . ?
C14 P5 C15 105.2(2) . . ?
C13 P5 C15 104.2(2) . . ?
C14 P5 Al2 116.89(16) . . ?
C13 P5 Al2 119.54(16) . . ?
C15 P5 Al2 105.66(15) . . ?
C17 P6 C18 103.7(2) . . ?
C17 P6 C16 106.2(2) . . ?
C18 P6 C16 104.5(2) . . ?
C17 P6 Al2 117.58(15) . . ?
C18 P6 Al2 120.21(16) . . ?
C16 P6 Al2 103.27(15) . . ?
C19 P7 C20 104.2(2) . . ?
C19 P7 C21 106.4(2) . . ?
C20 P7 C21 103.1(2) . . ?
C19 P7 Al2 117.33(16) . . ?
C20 P7 Al2 118.89(17) . . ?
C21 P7 Al2 105.38(15) . . ?
C23 P8 C22 107.1(2) . . ?
C23 P8 C24 104.3(2) . . ?
C22 P8 C24 103.0(2) . . ?
C23 P8 Al2 117.95(16) . . ?
C22 P8 Al2 103.26(15) . . ?
C24 P8 Al2 119.58(16) . . ?
Cl3 Al2 Cl4 179.36(8) . . ?
Cl3 Al2 P8 92.97(5) . . ?
Cl4 Al2 P8 87.51(5) . . ?
Cl3 Al2 P6 88.60(5) . . ?
Cl4 Al2 P6 90.93(5) . . ?
P8 Al2 P6 178.39(6) . . ?
Cl3 Al2 P7 88.86(6) . . ?
Cl4 Al2 P7 90.78(5) . . ?
P8 Al2 P7 83.27(5) . . ?
P6 Al2 P7 97.13(6) . . ?
Cl3 Al2 P5 89.29(6) . . ?
Cl4 Al2 P5 91.08(5) . . ?
P8 Al2 P5 96.69(6) . . ?
P6 Al2 P5 82.97(5) . . ?
P7 Al2 P5 178.14(6) . . ?
P5 C13 H13A 109.5 . . ?
P5 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
P5 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
P5 C14 H14A 109.5 . . ?
P5 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
P5 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C16 C15 P5 112.2(3) . . ?
C16 C15 H15A 109.2 . . ?
P5 C15 H15A 109.2 . . ?
C16 C15 H15B 109.2 . . ?
P5 C15 H15B 109.2 . . ?
H15A C15 H15B 107.9 . . ?
C15 C16 P6 111.5(3) . . ?
C15 C16 H16A 109.3 . . ?
P6 C16 H16A 109.3 . . ?
C15 C16 H16B 109.3 . . ?
P6 C16 H16B 109.3 . . ?
H16A C16 H16B 108.0 . . ?
P6 C17 H17A 109.5 . . ?
P6 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
P6 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
P6 C18 H18A 109.5 . . ?
P6 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
P6 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
P7 C19 H19A 109.5 . . ?
P7 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
P7 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
P7 C20 H20A 109.5 . . ?
P7 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
P7 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C22 C21 P7 113.1(3) . . ?
C22 C21 H21A 109.0 . . ?
P7 C21 H21A 109.0 . . ?
C22 C21 H21B 109.0 . . ?
P7 C21 H21B 109.0 . . ?
H21A C21 H21B 107.8 . . ?
C21 C22 P8 112.2(3) . . ?
C21 C22 H22A 109.2 . . ?
P8 C22 H22A 109.2 . . ?
C21 C22 H22B 109.2 . . ?
P8 C22 H22B 109.2 . . ?
H22A C22 H22B 107.9 . . ?
P8 C23 H23A 109.5 . . ?
P8 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
P8 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
P8 C24 H24A 109.5 . . ?
P8 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
P8 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
Cl5 Al3 Cl7 110.34(8) . . ?
Cl5 Al3 Cl6 111.69(8) . . ?
Cl7 Al3 Cl6 108.70(7) . . ?
Cl5 Al3 Cl8 108.29(8) . . ?
Cl7 Al3 Cl8 108.69(7) . . ?
Cl6 Al3 Cl8 109.07(8) . . ?
Cl11 Al4 Cl10 112.43(8) . . ?
Cl11 Al4 Cl12 108.00(8) . . ?
Cl10 Al4 Cl12 109.88(8) . . ?
Cl11 Al4 Cl9 109.56(8) . . ?
Cl10 Al4 Cl9 108.73(8) . . ?
Cl12 Al4 Cl9 108.15(7) . . ?

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
C6 P2 Al1 Cl1 137.80(16) . . . . ?
C5 P2 Al1 Cl1 10.46(18) . . . . ?
C4 P2 Al1 Cl1 -105.96(16) . . . . ?
C6 P2 Al1 Cl2 -42.24(16) . . . . ?
C5 P2 Al1 Cl2 -169.58(17) . . . . ?
C4 P2 Al1 Cl2 73.99(15) . . . . ?
C6 P2 Al1 P3 48.57(16) . . . . ?
C5 P2 Al1 P3 -78.77(17) . . . . ?
C4 P2 Al1 P3 164.81(15) . . . . ?
C6 P2 Al1 P4 -32.3(12) . . . . ?
C5 P2 Al1 P4 -159.6(11) . . . . ?
C4 P2 Al1 P4 84.0(11) . . . . ?
C6 P2 Al1 P1 -132.93(16) . . . . ?
C5 P2 Al1 P1 99.73(17) . . . . ?
C4 P2 Al1 P1 -16.69(15) . . . . ?
C7 P3 Al1 Cl1 -39.46(17) . . . . ?
C8 P3 Al1 Cl1 -166.83(18) . . . . ?
C9 P3 Al1 Cl1 77.86(15) . . . . ?
C7 P3 Al1 Cl2 140.38(17) . . . . ?
C8 P3 Al1 Cl2 13.01(18) . . . . ?
C9 P3 Al1 Cl2 -102.30(15) . . . . ?
C7 P3 Al1 P2 52.41(18) . . . . ?
C8 P3 Al1 P2 -74.96(18) . . . . ?
C9 P3 Al1 P2 169.73(14) . . . . ?
C7 P3 Al1 P4 -130.93(17) . . . . ?
C8 P3 Al1 P4 101.70(18) . . . . ?
C9 P3 Al1 P4 -13.61(14) . . . . ?
C7 P3 Al1 P1 -16(3) . . . . ?
C8 P3 Al1 P1 -144(2) . . . . ?
C9 P3 Al1 P1 101(2) . . . . ?
C11 P4 Al1 Cl1 144.14(17) . . . . ?
C12 P4 Al1 Cl1 14.65(18) . . . . ?
C10 P4 Al1 Cl1 -101.18(15) . . . . ?
C11 P4 Al1 Cl2 -35.82(17) . . . . ?
C12 P4 Al1 Cl2 -165.31(18) . . . . ?
C10 P4 Al1 Cl2 78.86(15) . . . . ?
C11 P4 Al1 P2 -45.8(12) . . . . ?
C12 P4 Al1 P2 -175.3(11) . . . . ?
C10 P4 Al1 P2 68.9(11) . . . . ?
C11 P4 Al1 P3 -126.99(17) . . . . ?
C12 P4 Al1 P3 103.53(18) . . . . ?
C10 P4 Al1 P3 -12.30(15) . . . . ?
C11 P4 Al1 P1 54.48(18) . . . . ?
C12 P4 Al1 P1 -75.01(18) . . . . ?
C10 P4 Al1 P1 169.16(15) . . . . ?
C1 P1 Al1 Cl1 -160.8(2) . . . . ?
C2 P1 Al1 Cl1 -32.50(19) . . . . ?
C3 P1 Al1 Cl1 83.76(16) . . . . ?
C1 P1 Al1 Cl2 19.3(2) . . . . ?
C2 P1 Al1 Cl2 147.66(18) . . . . ?
C3 P1 Al1 Cl2 -96.08(16) . . . . ?
C1 P1 Al1 P2 107.1(2) . . . . ?
C2 P1 Al1 P2 -124.53(18) . . . . ?
C3 P1 Al1 P2 -8.27(16) . . . . ?
C1 P1 Al1 P3 176(100) . . . . ?
C2 P1 Al1 P3 -56(2) . . . . ?
C3 P1 Al1 P3 61(2) . . . . ?
C1 P1 Al1 P4 -69.5(2) . . . . ?
C2 P1 Al1 P4 58.80(19) . . . . ?
C3 P1 Al1 P4 175.06(15) . . . . ?
C1 P1 C3 C4 -85.1(3) . . . . ?
C2 P1 C3 C4 164.5(3) . . . . ?
Al1 P1 C3 C4 38.8(3) . . . . ?
P1 C3 C4 P2 -57.7(4) . . . . ?
C6 P2 C4 C3 170.4(3) . . . . ?
C5 P2 C4 C3 -78.6(3) . . . . ?
Al1 P2 C4 C3 45.9(3) . . . . ?
C7 P3 C9 C10 169.4(3) . . . . ?
C8 P3 C9 C10 -79.8(3) . . . . ?
Al1 P3 C9 C10 44.2(3) . . . . ?
P3 C9 C10 P4 -60.0(3) . . . . ?
C11 P4 C10 C9 168.7(3) . . . . ?
C12 P4 C10 C9 -80.9(3) . . . . ?
Al1 P4 C10 C9 43.3(3) . . . . ?
C23 P8 Al2 Cl3 -7.4(2) . . . . ?
C22 P8 Al2 Cl3 110.47(17) . . . . ?
C24 P8 Al2 Cl3 -136.0(2) . . . . ?
C23 P8 Al2 Cl4 173.0(2) . . . . ?
C22 P8 Al2 Cl4 -69.11(17) . . . . ?
C24 P8 Al2 Cl4 44.5(2) . . . . ?
C23 P8 Al2 P6 160(2) . . . . ?
C22 P8 Al2 P6 -82(2) . . . . ?
C24 P8 Al2 P6 31(2) . . . . ?
C23 P8 Al2 P7 -95.9(2) . . . . ?
C22 P8 Al2 P7 21.97(16) . . . . ?
C24 P8 Al2 P7 135.5(2) . . . . ?
C23 P8 Al2 P5 82.2(2) . . . . ?
C22 P8 Al2 P5 -159.90(16) . . . . ?
C24 P8 Al2 P5 -46.3(2) . . . . ?
C17 P6 Al2 Cl3 -174.72(19) . . . . ?
C18 P6 Al2 Cl3 -47.0(2) . . . . ?
C16 P6 Al2 Cl3 68.79(17) . . . . ?
C17 P6 Al2 Cl4 4.86(19) . . . . ?
C18 P6 Al2 Cl4 132.6(2) . . . . ?
C16 P6 Al2 Cl4 -111.64(17) . . . . ?
C17 P6 Al2 P8 18(2) . . . . ?
C18 P6 Al2 P8 146(2) . . . . ?
C16 P6 Al2 P8 -98(2) . . . . ?
C17 P6 Al2 P7 -86.05(19) . . . . ?
C18 P6 Al2 P7 41.7(2) . . . . ?
C16 P6 Al2 P7 157.46(16) . . . . ?
C17 P6 Al2 P5 95.82(19) . . . . ?
C18 P6 Al2 P5 -136.4(2) . . . . ?
C16 P6 Al2 P5 -20.67(17) . . . . ?
C19 P7 Al2 Cl3 149.47(19) . . . . ?
C20 P7 Al2 Cl3 22.54(18) . . . . ?
C21 P7 Al2 Cl3 -92.34(17) . . . . ?
C19 P7 Al2 Cl4 -30.01(19) . . . . ?
C20 P7 Al2 Cl4 -156.94(18) . . . . ?
C21 P7 Al2 Cl4 88.18(17) . . . . ?
C19 P7 Al2 P8 -117.41(19) . . . . ?
C20 P7 Al2 P8 115.66(18) . . . . ?
C21 P7 Al2 P8 0.78(17) . . . . ?
C19 P7 Al2 P6 61.02(19) . . . . ?
C20 P7 Al2 P6 -65.91(18) . . . . ?
C21 P7 Al2 P6 179.21(17) . . . . ?
C19 P7 Al2 P5 154.0(19) . . . . ?
C20 P7 Al2 P5 27(2) . . . . ?
C21 P7 Al2 P5 -87.8(19) . . . . ?
C14 P5 Al2 Cl3 24.66(18) . . . . ?
C13 P5 Al2 Cl3 151.18(18) . . . . ?
C15 P5 Al2 Cl3 -91.97(16) . . . . ?
C14 P5 Al2 Cl4 -155.86(18) . . . . ?
C13 P5 Al2 Cl4 -29.34(19) . . . . ?
C15 P5 Al2 Cl4 87.50(16) . . . . ?
C14 P5 Al2 P8 -68.24(18) . . . . ?
C13 P5 Al2 P8 58.27(19) . . . . ?
C15 P5 Al2 P8 175.12(16) . . . . ?
C14 P5 Al2 P6 113.34(18) . . . . ?
C13 P5 Al2 P6 -120.15(18) . . . . ?
C15 P5 Al2 P6 -3.30(16) . . . . ?
C14 P5 Al2 P7 20(2) . . . . ?
C13 P5 Al2 P7 146.6(19) . . . . ?
C15 P5 Al2 P7 -96.5(19) . . . . ?
C14 P5 C15 C16 -91.0(3) . . . . ?
C13 P5 C15 C16 160.1(3) . . . . ?
Al2 P5 C15 C16 33.3(3) . . . . ?
P5 C15 C16 P6 -55.9(4) . . . . ?
C17 P6 C16 C15 -75.9(3) . . . . ?
C18 P6 C16 C15 174.9(3) . . . . ?
Al2 P6 C16 C15 48.4(3) . . . . ?
C19 P7 C21 C22 95.4(4) . . . . ?
C20 P7 C21 C22 -155.2(3) . . . . ?
Al2 P7 C21 C22 -29.9(4) . . . . ?
P7 C21 C22 P8 53.6(4) . . . . ?
C23 P8 C22 C21 77.0(4) . . . . ?
C24 P8 C22 C21 -173.3(3) . . . . ?
Al2 P8 C22 C21 -48.2(3) . . . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.850
_refine_diff_density_min         -0.460
_refine_diff_density_rms         0.095
_database_code_depnum_ccdc_archive 'CCDC 1005865'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_[(AlCl3)2{?-Cy2P(CH2)2PCy2}]
#data_13jebr16a

_audit_creation_method           'SHELXL-97 + hand edit'
_chemical_name_systematic        
;
 1,2-bis(dicyclohexylphosphino)ethane-bis(trichloroaluminium)
;


# (C6H11)2PCH2CH2P(C6H11)2 = C26H48P2 = Cy2P(CH2)2PCy2
# ethane-1,2-diylbis(dicyclohexylphosphane) (Chemspider)
# 1,2-ethanediylbis(dicyclohexylphosphine)  (Chemspider) 
# 1,2-bis(dicyclohexylphosphino)ethane  (Chemspider alternative)

_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C26 H48 Al2 Cl6 P2'
_chemical_formula_sum            'C26 H48 Al2 Cl6 P2'
_chemical_formula_weight         689.24

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'
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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_name_H-M_alt        'P -1'
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.251(2)
_cell_length_b                   9.830(2)
_cell_length_c                   11.921(3)
_cell_angle_alpha                113.905(8)
_cell_angle_beta                 91.329(6)
_cell_angle_gamma                103.390(7)
_cell_volume                     852.4(4)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    5445
_cell_measurement_theta_min      3.2
_cell_measurement_theta_max      27.5 # new theta_max value

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.343
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             362
_exptl_absorpt_coefficient_mu    0.666
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9487
_exptl_absorpt_correction_T_max  0.9739
_exptl_absorpt_process_details   'CrystalClear-SM Expert 2.0 r11 (Rigaku, 2011)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source_power             2.5
_diffrn_source_voltage           45.0
_diffrn_source_current           55.0
_diffrn_source                   'Rotating Anode'
_diffrn_radiation_monochromator  Confocal
_diffrn_measurement_specimen_support Mitegen
_diffrn_detector                 CCD
_diffrn_measurement_device       
;
AFC12 (Right): Kappa 3 circle
;
_diffrn_measurement_device_type  
;
Rigaku Saturn724+ (2x2 bin mode)
;
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            8428
_diffrn_reflns_av_R_equivalents  0.1141
_diffrn_reflns_av_sigmaI/netI    0.1743
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.97
_diffrn_reflns_theta_max         27.48
_reflns_number_total             3884
_reflns_number_gt                2038
_reflns_threshold_expression     >2σ(I)

_computing_data_collection       
;
CrystalClear-SM Expert 2.0 r11 (Rigaku, 2011)
;
_computing_cell_refinement       
;
CrystalClear-SM Expert 2.0 r11 (Rigaku, 2011)
;
_computing_data_reduction        
;
CrystalClear-SM Expert 2.0 r11 (Rigaku, 2011)
;
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0919P)²+0.4637P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3884
_refine_ls_number_parameters     163
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1743
_refine_ls_R_factor_gt           0.0859
_refine_ls_wR_factor_ref         0.2276
_refine_ls_wR_factor_gt          0.1751
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_restrained_S_all      1.035
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Al1 Al 1.2517(2) 0.3772(2) 0.26994(19) 0.0222(5) Uani 1 1 d . . .
Cl1 Cl 1.2651(2) 0.2638(2) 0.07764(16) 0.0285(4) Uani 1 1 d . . .
Cl2 Cl 1.3125(2) 0.6213(2) 0.33357(17) 0.0283(4) Uani 1 1 d . . .
Cl3 Cl 1.3878(2) 0.3049(2) 0.37802(18) 0.0334(5) Uani 1 1 d . . .
P1 P 0.9634(2) 0.31430(19) 0.30502(16) 0.0184(4) Uani 1 1 d . . .
C1 C 0.8110(8) 0.2983(7) 0.1824(6) 0.0193(14) Uani 1 1 d . . .
H1 H 0.6999 0.2979 0.2142 0.023 Uiso 1 1 calc R . .
C2 C 0.8646(8) 0.4402(8) 0.1527(6) 0.0235(15) Uani 1 1 d . . .
H2A H 0.8731 0.5353 0.2286 0.028 Uiso 1 1 calc R . .
H2B H 0.9767 0.4456 0.1242 0.028 Uiso 1 1 calc R . .
C3 C 0.7370(9) 0.4304(8) 0.0518(7) 0.0288(17) Uani 1 1 d . . .
H3A H 0.6273 0.4345 0.0831 0.035 Uiso 1 1 calc R . .
H3B H 0.7763 0.5197 0.0314 0.035 Uiso 1 1 calc R . .
C4 C 0.7156(9) 0.2808(9) -0.0646(7) 0.0309(17) Uani 1 1 d . . .
H4A H 0.6288 0.2743 -0.1267 0.037 Uiso 1 1 calc R . .
H4B H 0.8227 0.2821 -0.1004 0.037 Uiso 1 1 calc R . .
C5 C 0.6650(9) 0.1409(8) -0.0376(6) 0.0268(16) Uani 1 1 d . . .
H5A H 0.6594 0.0473 -0.1143 0.032 Uiso 1 1 calc R . .
H5B H 0.5514 0.1327 -0.0115 0.032 Uiso 1 1 calc R . .
C6 C 0.7884(9) 0.1474(8) 0.0643(6) 0.0232(15) Uani 1 1 d . . .
H6A H 0.8986 0.1415 0.0343 0.028 Uiso 1 1 calc R . .
H6B H 0.7454 0.0579 0.0838 0.028 Uiso 1 1 calc R . .
C7 C 0.9038(8) 0.1452(7) 0.3403(6) 0.0203(14) Uani 1 1 d . . .
H7 H 0.9610 0.1792 0.4258 0.024 Uiso 1 1 calc R . .
C8 C 0.7144(8) 0.0927(8) 0.3468(6) 0.0227(15) Uani 1 1 d . . .
H8A H 0.6774 0.1806 0.4064 0.027 Uiso 1 1 calc R . .
H8B H 0.6504 0.0584 0.2645 0.027 Uiso 1 1 calc R . .
C9 C 0.6779(9) -0.0382(8) 0.3865(7) 0.0273(16) Uani 1 1 d . . .
H9A H 0.7309 0.0004 0.4728 0.033 Uiso 1 1 calc R . .
H9B H 0.5550 -0.0742 0.3846 0.033 Uiso 1 1 calc R . .
C10 C 0.7423(9) -0.1728(8) 0.3045(7) 0.0301(17) Uani 1 1 d . . .
H10A H 0.6800 -0.2197 0.2200 0.036 Uiso 1 1 calc R . .
H10B H 0.7224 -0.2522 0.3373 0.036 Uiso 1 1 calc R . .
C11 C 0.9294(9) -0.1201(8) 0.2987(7) 0.0267(16) Uani 1 1 d . . .
H11A H 0.9922 -0.0841 0.3817 0.032 Uiso 1 1 calc R . .
H11B H 0.9670 -0.2089 0.2410 0.032 Uiso 1 1 calc R . .
C12 C 0.9704(8) 0.0088(7) 0.2565(6) 0.0218(14) Uani 1 1 d . . .
H12A H 0.9186 -0.0300 0.1698 0.026 Uiso 1 1 calc R . .
H12B H 1.0936 0.0441 0.2596 0.026 Uiso 1 1 calc R . .
C13 C 0.9363(8) 0.4775(7) 0.4428(5) 0.0181(14) Uani 1 1 d . . .
H13A H 0.9479 0.5678 0.4234 0.022 Uiso 1 1 calc R . .
H13B H 0.8211 0.4508 0.4634 0.022 Uiso 1 1 calc R . .


_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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
Al1 Cl3 2.114(3) . ?
Al1 Cl1 2.123(3) . ?
Al1 Cl2 2.129(3) . ?
Al1 P1 2.407(3) . ?
P1 C13 1.836(6) . ?
P1 C1 1.839(6) . ?
P1 C7 1.839(6) . ?
C1 C6 1.544(9) . ?
C1 C2 1.545(9) . ?
C1 H1 1.0000 . ?
C2 C3 1.538(9) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.527(10) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 C5 1.506(10) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C6 1.538(9) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C8 1.542(9) . ?
C7 C12 1.543(9) . ?
C7 H7 1.0000 . ?
C8 C9 1.514(9) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C10 1.513(10) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 C11 1.523(10) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C12 1.516(9) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 C13 1.546(12) 2_766 ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?

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 Al1 Cl1 112.98(12) . . ?
Cl3 Al1 Cl2 113.23(12) . . ?
Cl1 Al1 Cl2 112.00(12) . . ?
Cl3 Al1 P1 106.20(11) . . ?
Cl1 Al1 P1 108.76(11) . . ?
Cl2 Al1 P1 102.90(10) . . ?
C13 P1 C1 104.0(3) . . ?
C13 P1 C7 105.7(3) . . ?
C1 P1 C7 110.8(3) . . ?
C13 P1 Al1 107.3(2) . . ?
C1 P1 Al1 114.1(2) . . ?
C7 P1 Al1 114.0(2) . . ?
C6 C1 C2 110.7(5) . . ?
C6 C1 P1 112.2(4) . . ?
C2 C1 P1 110.0(4) . . ?
C6 C1 H1 107.9 . . ?
C2 C1 H1 107.9 . . ?
P1 C1 H1 107.9 . . ?
C3 C2 C1 110.8(5) . . ?
C3 C2 H2A 109.5 . . ?
C1 C2 H2A 109.5 . . ?
C3 C2 H2B 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 108.1 . . ?
C4 C3 C2 110.5(6) . . ?
C4 C3 H3A 109.5 . . ?
C2 C3 H3A 109.5 . . ?
C4 C3 H3B 109.5 . . ?
C2 C3 H3B 109.5 . . ?
H3A C3 H3B 108.1 . . ?
C5 C4 C3 111.9(6) . . ?
C5 C4 H4A 109.2 . . ?
C3 C4 H4A 109.2 . . ?
C5 C4 H4B 109.2 . . ?
C3 C4 H4B 109.2 . . ?
H4A C4 H4B 107.9 . . ?
C4 C5 C6 112.4(6) . . ?
C4 C5 H5A 109.1 . . ?
C6 C5 H5A 109.1 . . ?
C4 C5 H5B 109.1 . . ?
C6 C5 H5B 109.1 . . ?
H5A C5 H5B 107.9 . . ?
C5 C6 C1 110.6(5) . . ?
C5 C6 H6A 109.5 . . ?
C1 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
C1 C6 H6B 109.5 . . ?
H6A C6 H6B 108.1 . . ?
C8 C7 C12 111.4(5) . . ?
C8 C7 P1 114.0(4) . . ?
C12 C7 P1 113.6(5) . . ?
C8 C7 H7 105.7 . . ?
C12 C7 H7 105.7 . . ?
P1 C7 H7 105.7 . . ?
C9 C8 C7 110.7(5) . . ?
C9 C8 H8A 109.5 . . ?
C7 C8 H8A 109.5 . . ?
C9 C8 H8B 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 108.1 . . ?
C10 C9 C8 112.5(6) . . ?
C10 C9 H9A 109.1 . . ?
C8 C9 H9A 109.1 . . ?
C10 C9 H9B 109.1 . . ?
C8 C9 H9B 109.1 . . ?
H9A C9 H9B 107.8 . . ?
C9 C10 C11 110.7(6) . . ?
C9 C10 H10A 109.5 . . ?
C11 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
C11 C10 H10B 109.5 . . ?
H10A C10 H10B 108.1 . . ?
C12 C11 C10 112.4(6) . . ?
C12 C11 H11A 109.1 . . ?
C10 C11 H11A 109.1 . . ?
C12 C11 H11B 109.1 . . ?
C10 C11 H11B 109.1 . . ?
H11A C11 H11B 107.9 . . ?
C11 C12 C7 110.3(5) . . ?
C11 C12 H12A 109.6 . . ?
C7 C12 H12A 109.6 . . ?
C11 C12 H12B 109.6 . . ?
C7 C12 H12B 109.6 . . ?
H12A C12 H12B 108.1 . . ?
C13 C13 P1 113.5(6) 2_766 . ?
C13 C13 H13A 108.9 2_766 . ?
P1 C13 H13A 108.9 . . ?
C13 C13 H13B 108.9 2_766 . ?
P1 C13 H13B 108.9 . . ?
H13A C13 H13B 107.7 . . ?

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
Cl3 Al1 P1 C13 86.9(2) . . . . ?
Cl1 Al1 P1 C13 -151.2(2) . . . . ?
Cl2 Al1 P1 C13 -32.3(2) . . . . ?
Cl3 Al1 P1 C1 -158.5(2) . . . . ?
Cl1 Al1 P1 C1 -36.6(3) . . . . ?
Cl2 Al1 P1 C1 82.3(3) . . . . ?
Cl3 Al1 P1 C7 -29.8(3) . . . . ?
Cl1 Al1 P1 C7 92.1(3) . . . . ?
Cl2 Al1 P1 C7 -149.0(3) . . . . ?
C13 P1 C1 C6 -168.6(5) . . . . ?
C7 P1 C1 C6 -55.5(6) . . . . ?
Al1 P1 C1 C6 74.8(5) . . . . ?
C13 P1 C1 C2 67.7(5) . . . . ?
C7 P1 C1 C2 -179.2(4) . . . . ?
Al1 P1 C1 C2 -48.9(5) . . . . ?
C6 C1 C2 C3 56.4(7) . . . . ?
P1 C1 C2 C3 -179.0(5) . . . . ?
C1 C2 C3 C4 -56.6(8) . . . . ?
C2 C3 C4 C5 56.1(8) . . . . ?
C3 C4 C5 C6 -55.4(8) . . . . ?
C4 C5 C6 C1 54.5(8) . . . . ?
C2 C1 C6 C5 -54.7(7) . . . . ?
P1 C1 C6 C5 -178.0(5) . . . . ?
C13 P1 C7 C8 69.6(5) . . . . ?
C1 P1 C7 C8 -42.5(6) . . . . ?
Al1 P1 C7 C8 -172.8(4) . . . . ?
C13 P1 C7 C12 -161.3(5) . . . . ?
C1 P1 C7 C12 86.6(5) . . . . ?
Al1 P1 C7 C12 -43.7(5) . . . . ?
C12 C7 C8 C9 54.5(7) . . . . ?
P1 C7 C8 C9 -175.3(5) . . . . ?
C7 C8 C9 C10 -55.1(8) . . . . ?
C8 C9 C10 C11 55.4(8) . . . . ?
C9 C10 C11 C12 -55.7(8) . . . . ?
C10 C11 C12 C7 55.5(8) . . . . ?
C8 C7 C12 C11 -54.7(7) . . . . ?
P1 C7 C12 C11 174.9(5) . . . . ?
C1 P1 C13 C13 -175.1(6) . . . 2_766 ?
C7 P1 C13 C13 68.2(7) . . . 2_766 ?
Al1 P1 C13 C13 -53.9(7) . . . 2_766 ?

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         0.826
_refine_diff_density_min         -0.512
_refine_diff_density_rms         0.142
_database_code_depnum_ccdc_archive 'CCDC 1005866'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_[o-C6H4(AsMe2)2(CH2)][AlCl4]2
#data_j24

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C11 H18 As2, 2(Al Cl4 1-)'
_chemical_formula_sum            'C11 H18 Al2 As2 Cl8'
_chemical_formula_weight         637.65

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'
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'
As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_name_H-M_alt        Pna21
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'

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

_cell_length_a                   14.7537(10)
_cell_length_b                   14.9361(10)
_cell_length_c                   10.9633(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2415.9(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    19941
_cell_measurement_theta_min      3.06
_cell_measurement_theta_max      27.48

_exptl_crystal_description       chunk
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.753
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1248
_exptl_absorpt_coefficient_mu    3.719
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7074
_exptl_absorpt_correction_T_max  0.8077
_exptl_absorpt_process_details   'CrystalClear-SM Expert 2.0 r11 (Rigaku, 2011)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source_power             2.5
_diffrn_source_voltage           45.0
_diffrn_source_current           55.0
_diffrn_source                   'Rotating Anode'
_diffrn_radiation_monochromator  Confocal
_diffrn_measurement_specimen_support Mitegen
_diffrn_detector                 CCD
_diffrn_measurement_device       
;
AFC12 (Right): Kappa 3 circle
;
_diffrn_measurement_device_type  
;
Rigaku Saturn724+ (2x2 bin mode)
;
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            19941
_diffrn_reflns_av_R_equivalents  0.0490
_diffrn_reflns_av_sigmaI/netI    0.0396
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         3.06
_diffrn_reflns_theta_max         27.48
_reflns_number_total             4813
_reflns_number_gt                4284
_reflns_threshold_expression     >2σ(I)

_computing_data_collection       
;
CrystalClear-SM Expert 2.0 r11 (Rigaku, 2011)
;
_computing_cell_refinement       
;
CrystalClear-SM Expert 2.0 r11 (Rigaku, 2011)
;
_computing_data_reduction        
;
CrystalClear-SM Expert 2.0 r11 (Rigaku, 2011)
;
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.

 PLAT241_ALERT_2_C High      Ueq as Compared to Neighbors for C11 Check 
 PLAT242_ALERT_2_C Low       Ueq as Compared to Neighbors for Al1 Check 
 PLAT242_ALERT_2_C Low       Ueq as Compared to Neighbors for Al2 Check 

 The above 3 atoms are all bonded and C11 has a small amount of positional 
 freedom and as a result shows a slightly elevated degree of thermal motion 
 compared to the aluminiums.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0536P)²+3.3503P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.241(11)
_refine_ls_number_reflns         4813
_refine_ls_number_parameters     213
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0499
_refine_ls_R_factor_gt           0.0409
_refine_ls_wR_factor_ref         0.1002
_refine_ls_wR_factor_gt          0.0954
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_restrained_S_all      1.040
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
As1 As 0.20268(3) 0.98070(3) 0.75346(6) 0.02952(14) Uani 1 1 d . . .
As2 As 0.35568(4) 0.91172(4) 0.58290(5) 0.02634(13) Uani 1 1 d . . .
Cl6 Cl 0.86133(10) 1.49199(9) 1.24275(15) 0.0381(3) Uani 1 1 d . . .
Cl2 Cl 0.46461(10) 1.17455(10) 0.76876(17) 0.0427(4) Uani 1 1 d . . .
Al1 Al 0.43171(11) 1.31407(11) 0.76131(18) 0.0311(4) Uani 1 1 d . . .
Cl3 Cl 0.47273(12) 1.37893(11) 0.92605(14) 0.0421(4) Uani 1 1 d . . .
Al2 Al 0.78435(11) 1.37202(11) 1.24371(19) 0.0326(4) Uani 1 1 d . . .
Cl7 Cl 0.84624(12) 1.27976(13) 1.12141(18) 0.0581(6) Uani 1 1 d . . .
Cl1 Cl 0.29069(11) 1.32519(12) 0.7392(3) 0.0635(6) Uani 1 1 d . . .
Cl5 Cl 0.65060(12) 1.39648(15) 1.1838(3) 0.0729(7) Uani 1 1 d . . .
Cl4 Cl 0.50206(15) 1.37548(13) 0.61236(15) 0.0540(5) Uani 1 1 d . . .
Cl8 Cl 0.79150(16) 1.31824(13) 1.42435(19) 0.0639(6) Uani 1 1 d . . .
C10 C 0.3656(3) 0.8818(3) 0.7515(5) 0.0217(9) Uani 1 1 d . . .
C5 C 0.2985(4) 0.9150(3) 0.8290(5) 0.0235(11) Uani 1 1 d . . .
C6 C 0.3027(4) 0.8985(4) 0.9540(5) 0.0299(12) Uani 1 1 d . . .
H6 H 0.2573 0.9208 1.0074 0.036 Uiso 1 1 calc R . .
C11 C 0.2356(4) 0.9692(5) 0.5802(7) 0.0436(15) Uani 1 1 d . . .
H13A H 0.2387 1.0287 0.5406 0.052 Uiso 1 1 calc R . .
H13B H 0.1911 0.9316 0.5362 0.052 Uiso 1 1 calc R . .
C2 C 0.0875(4) 0.9275(4) 0.7847(6) 0.0381(15) Uani 1 1 d . . .
H4A H 0.0399 0.9632 0.7458 0.057 Uiso 1 1 calc R . .
H4B H 0.0770 0.9252 0.8729 0.057 Uiso 1 1 calc R . .
H4C H 0.0866 0.8666 0.7514 0.057 Uiso 1 1 calc R . .
C9 C 0.4376(4) 0.8317(4) 0.7970(5) 0.0279(12) Uani 1 1 d . . .
H3 H 0.4835 0.8093 0.7444 0.034 Uiso 1 1 calc R . .
C4 C 0.3605(6) 0.8064(5) 0.4843(6) 0.051(2) Uani 1 1 d . . .
H2A H 0.3043 0.7722 0.4944 0.076 Uiso 1 1 calc R . .
H2B H 0.4122 0.7695 0.5093 0.076 Uiso 1 1 calc R . .
H2C H 0.3675 0.8235 0.3985 0.076 Uiso 1 1 calc R . .
C3 C 0.4501(5) 0.9928(4) 0.5396(6) 0.0372(14) Uani 1 1 d . . .
H1A H 0.5088 0.9625 0.5461 0.056 Uiso 1 1 calc R . .
H1B H 0.4490 1.0444 0.5948 0.056 Uiso 1 1 calc R . .
H1C H 0.4411 1.0133 0.4555 0.056 Uiso 1 1 calc R . .
C8 C 0.4403(4) 0.8154(4) 0.9214(6) 0.0322(13) Uani 1 1 d . . .
H11 H 0.4881 0.7804 0.9544 0.039 Uiso 1 1 calc R . .
C7 C 0.3745(4) 0.8492(4) 0.9979(5) 0.0324(14) Uani 1 1 d . . .
H10 H 0.3788 0.8381 1.0830 0.039 Uiso 1 1 calc R . .
C1 C 0.2086(5) 1.1029(4) 0.8043(9) 0.058(2) Uani 1 1 d . . .
H9A H 0.2712 1.1242 0.7981 0.087 Uiso 1 1 calc R . .
H9B H 0.1881 1.1077 0.8891 0.087 Uiso 1 1 calc R . .
H9C H 0.1694 1.1394 0.7519 0.087 Uiso 1 1 calc R . .


_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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
As1 C2 1.907(6) . ?
As1 C5 1.910(5) . ?
As1 C1 1.910(7) . ?
As1 C11 1.968(7) . ?
As2 C3 1.906(6) . ?
As2 C10 1.907(5) . ?
As2 C4 1.910(7) . ?
As2 C11 1.969(7) . ?
Cl6 Al2 2.122(2) . ?
Cl2 Al1 2.141(2) . ?
Al1 Cl1 2.101(2) . ?
Al1 Cl3 2.137(2) . ?
Al1 Cl4 2.141(3) . ?
Al2 Cl5 2.112(2) . ?
Al2 Cl7 2.128(2) . ?
Al2 Cl8 2.140(3) . ?
C10 C9 1.391(7) . ?
C10 C5 1.396(7) . ?
C5 C6 1.393(8) . ?
C6 C7 1.378(8) . ?
C6 H6 0.9500 . ?
C11 H13A 0.9900 . ?
C11 H13B 0.9900 . ?
C2 H4A 0.9800 . ?
C2 H4B 0.9800 . ?
C2 H4C 0.9800 . ?
C9 C8 1.386(8) . ?
C9 H3 0.9500 . ?
C4 H2A 0.9800 . ?
C4 H2B 0.9800 . ?
C4 H2C 0.9800 . ?
C3 H1A 0.9800 . ?
C3 H1B 0.9800 . ?
C3 H1C 0.9800 . ?
C8 C7 1.378(9) . ?
C8 H11 0.9500 . ?
C7 H10 0.9500 . ?
C1 H9A 0.9800 . ?
C1 H9B 0.9800 . ?
C1 H9C 0.9800 . ?

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
C2 As1 C5 111.5(3) . . ?
C2 As1 C1 112.7(3) . . ?
C5 As1 C1 109.3(3) . . ?
C2 As1 C11 110.9(3) . . ?
C5 As1 C11 101.0(3) . . ?
C1 As1 C11 110.7(4) . . ?
C3 As2 C10 109.5(2) . . ?
C3 As2 C4 110.8(3) . . ?
C10 As2 C4 110.7(3) . . ?
C3 As2 C11 112.1(3) . . ?
C10 As2 C11 100.7(2) . . ?
C4 As2 C11 112.6(3) . . ?
Cl1 Al1 Cl3 110.01(12) . . ?
Cl1 Al1 Cl2 107.81(9) . . ?
Cl3 Al1 Cl2 110.17(11) . . ?
Cl1 Al1 Cl4 110.98(12) . . ?
Cl3 Al1 Cl4 108.24(10) . . ?
Cl2 Al1 Cl4 109.64(10) . . ?
Cl5 Al2 Cl6 110.65(11) . . ?
Cl5 Al2 Cl7 108.49(11) . . ?
Cl6 Al2 Cl7 108.30(11) . . ?
Cl5 Al2 Cl8 113.51(14) . . ?
Cl6 Al2 Cl8 107.17(10) . . ?
Cl7 Al2 Cl8 108.59(12) . . ?
C9 C10 C5 121.0(5) . . ?
C9 C10 As2 122.1(4) . . ?
C5 C10 As2 116.9(4) . . ?
C6 C5 C10 120.3(5) . . ?
C6 C5 As1 123.4(4) . . ?
C10 C5 As1 116.3(4) . . ?
C7 C6 C5 118.2(5) . . ?
C7 C6 H6 120.9 . . ?
C5 C6 H6 120.9 . . ?
As1 C11 As2 104.2(3) . . ?
As1 C11 H13A 110.9 . . ?
As2 C11 H13A 110.9 . . ?
As1 C11 H13B 110.9 . . ?
As2 C11 H13B 110.9 . . ?
H13A C11 H13B 108.9 . . ?
As1 C2 H4A 109.5 . . ?
As1 C2 H4B 109.5 . . ?
H4A C2 H4B 109.5 . . ?
As1 C2 H4C 109.5 . . ?
H4A C2 H4C 109.5 . . ?
H4B C2 H4C 109.5 . . ?
C8 C9 C10 118.0(5) . . ?
C8 C9 H3 121.0 . . ?
C10 C9 H3 121.0 . . ?
As2 C4 H2A 109.5 . . ?
As2 C4 H2B 109.5 . . ?
H2A C4 H2B 109.5 . . ?
As2 C4 H2C 109.5 . . ?
H2A C4 H2C 109.5 . . ?
H2B C4 H2C 109.5 . . ?
As2 C3 H1A 109.5 . . ?
As2 C3 H1B 109.5 . . ?
H1A C3 H1B 109.5 . . ?
As2 C3 H1C 109.5 . . ?
H1A C3 H1C 109.5 . . ?
H1B C3 H1C 109.5 . . ?
C7 C8 C9 120.9(5) . . ?
C7 C8 H11 119.5 . . ?
C9 C8 H11 119.5 . . ?
C6 C7 C8 121.7(5) . . ?
C6 C7 H10 119.2 . . ?
C8 C7 H10 119.2 . . ?
As1 C1 H9A 109.5 . . ?
As1 C1 H9B 109.5 . . ?
H9A C1 H9B 109.5 . . ?
As1 C1 H9C 109.5 . . ?
H9A C1 H9C 109.5 . . ?
H9B C1 H9C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C3 As2 C10 C9 -67.6(5) . . . . ?
C4 As2 C10 C9 54.8(5) . . . . ?
C11 As2 C10 C9 174.1(4) . . . . ?
C3 As2 C10 C5 110.4(4) . . . . ?
C4 As2 C10 C5 -127.1(4) . . . . ?
C11 As2 C10 C5 -7.9(4) . . . . ?
C9 C10 C5 C6 0.2(8) . . . . ?
As2 C10 C5 C6 -177.9(4) . . . . ?
C9 C10 C5 As1 -178.9(4) . . . . ?
As2 C10 C5 As1 3.1(5) . . . . ?
C2 As1 C5 C6 -57.9(5) . . . . ?
C1 As1 C5 C6 67.4(6) . . . . ?
C11 As1 C5 C6 -175.8(5) . . . . ?
C2 As1 C5 C10 121.1(4) . . . . ?
C1 As1 C5 C10 -113.6(5) . . . . ?
C11 As1 C5 C10 3.2(4) . . . . ?
C10 C5 C6 C7 0.1(8) . . . . ?
As1 C5 C6 C7 179.1(4) . . . . ?
C2 As1 C11 As2 -125.8(3) . . . . ?
C5 As1 C11 As2 -7.4(3) . . . . ?
C1 As1 C11 As2 108.3(3) . . . . ?
C3 As2 C11 As1 -107.7(3) . . . . ?
C10 As2 C11 As1 8.7(3) . . . . ?
C4 As2 C11 As1 126.6(3) . . . . ?
C5 C10 C9 C8 0.3(8) . . . . ?
As2 C10 C9 C8 178.3(4) . . . . ?
C10 C9 C8 C7 -1.1(8) . . . . ?
C5 C6 C7 C8 -0.9(8) . . . . ?
C9 C8 C7 C6 1.5(8) . . . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.918
_refine_diff_density_min         -0.489
_refine_diff_density_rms         0.109
_database_code_depnum_ccdc_archive 'CCDC 1005867'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_[o-C6H4(PMe2)(PHMe2)]2[AlCl4][Cl]
#data_13jebr11 

_audit_creation_method           'SHELXL-97 + hand edit'
_audit_creation_date             2013-08-23 # yyyy-mm-dd

_chemical_name_systematic        
; 
 bis[(2-dimethylphosphanylphenyl)-dimethylphosphonium]
 tetrachloroaluminium(III) chloride
;

# [o-C6H4(PMe2)(P(H)Me2)]+ = [C10H17P2]+
# (2-dimethylphosphanylphenyl)-dimethylphosphonium
# benzene-1-yl(dimethylphosphane)-2-yl(dimethylphosphonium) 

_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C10 H17 P2 1+), Al Cl4 1-, Cl 1-'
_chemical_formula_sum            'C20 H34 Al Cl5 P4'
_chemical_formula_weight         602.58

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'
Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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_name_H-M_alt        'C 2/c'
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'



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

_cell_length_a                   14.599(5)
_cell_length_b                   20.672(7)
_cell_length_c                   11.006(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 115.061(5)
_cell_angle_gamma                90.00
_cell_volume                     3009(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    5094
_cell_measurement_theta_min      1.8
_cell_measurement_theta_max      34.7

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.330
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1248
_exptl_absorpt_coefficient_mu    0.733
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.671 # Expt'l Tmin & Tmax 
_exptl_absorpt_correction_T_max  1.000 # scaled to Tmax=1.0
_exptl_absorpt_process_details   
;Jacobson, R.A. (1998). REQAB. Private communication to the 
 Rigaku Corporation, Tokyo, Japan. 
;


_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  ?
_diffrn_radiation_collimation    'Confocal mirrors, VHF VariMax '

_diffrn_source                   'Rotating anode X-ray tube'
_diffrn_source_type              'Rigaku FR-E+ Superbright'

_diffrn_measurement_device       'Four-circle κ diffractometer'
_diffrn_measurement_device_type  'Rigaku AFC12 '
_diffrn_measurement_method       'Profile data from ω-scans'

_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Rigaku HG Saturn724+ (2x2 bin mode)'
_diffrn_detector_area_resol_mean ?

_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            18200
_diffrn_reflns_av_R_equivalents  0.0930
# _diffrn_reflns_av_sigmaI/netI   0.0780 
_diffrn_reflns_av_unetI/netI     0.0780
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         1.83
_diffrn_reflns_theta_max         27.50
_reflns_number_total             3461
_reflns_number_gt                2839
_reflns_threshold_expression     I>2σ(I)

_computing_data_collection       'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)'
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'ORTEP-III (Farrugia, 1997)'
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 

 Shelxl-97 refinement
 _refine_ls_hydrogen_treatment  constr for the C bonded H atoms.
 H1 bonded to P1 was very clear (Q1 in the difference map) and
 refined well without any restraints being imposed.  
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0318P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed # constr (C-H) refall (P-H)
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3461
_refine_ls_number_parameters     146
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0859
_refine_ls_R_factor_gt           0.0640
_refine_ls_wR_factor_ref         0.1111
_refine_ls_wR_factor_gt          0.1041
_refine_ls_goodness_of_fit_ref   1.158
_refine_ls_restrained_S_all      1.158
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
P1 P 0.16638(7) 0.05886(4) 0.37607(9) 0.0221(2) Uani 1 1 d . . .
P2 P 0.06356(7) 0.17899(5) 0.46278(9) 0.0246(2) Uani 1 1 d . . .
H1 H 0.070(2) 0.0590(15) 0.339(3) 0.031(10) Uiso 1 1 d . . .
C1 C 0.2300(2) 0.09400(15) 0.5403(3) 0.0167(7) Uani 1 1 d . . .
C2 C 0.1867(2) 0.14580(15) 0.5801(3) 0.0165(7) Uani 1 1 d . . .
C3 C 0.2401(3) 0.17078(16) 0.7092(3) 0.0213(7) Uani 1 1 d . . .
H3 H 0.2117 0.2053 0.7389 0.026 Uiso 1 1 calc R . .
C4 C 0.3333(2) 0.14640(17) 0.7944(3) 0.0228(8) Uani 1 1 d . . .
H4 H 0.3681 0.1642 0.8817 0.027 Uiso 1 1 calc R . .
C5 C 0.3762(3) 0.09627(17) 0.7536(3) 0.0239(8) Uani 1 1 d . . .
H5 H 0.4407 0.0800 0.8121 0.029 Uiso 1 1 calc R . .
C6 C 0.3247(3) 0.06982(16) 0.6269(3) 0.0237(8) Uani 1 1 d . . .
H6 H 0.3539 0.0351 0.5988 0.028 Uiso 1 1 calc R . .
C7 C 0.2072(3) -0.02186(17) 0.3731(4) 0.0410(11) Uani 1 1 d . . .
H7A H 0.1693 -0.0403 0.2836 0.061 Uiso 1 1 calc R . .
H7B H 0.1954 -0.0478 0.4395 0.061 Uiso 1 1 calc R . .
H7C H 0.2796 -0.0219 0.3945 0.061 Uiso 1 1 calc R . .
C8 C 0.1891(3) 0.10535(18) 0.2551(3) 0.0283(8) Uani 1 1 d . . .
H8A H 0.2618 0.1059 0.2786 0.042 Uiso 1 1 calc R . .
H8B H 0.1652 0.1497 0.2542 0.042 Uiso 1 1 calc R . .
H8C H 0.1529 0.0860 0.1662 0.042 Uiso 1 1 calc R . .
C9 C -0.0070(3) 0.17638(17) 0.5669(3) 0.0268(8) Uani 1 1 d . . .
H9A H -0.0181 0.1312 0.5844 0.040 Uiso 1 1 calc R . .
H9B H -0.0723 0.1980 0.5198 0.040 Uiso 1 1 calc R . .
H9C H 0.0319 0.1985 0.6522 0.040 Uiso 1 1 calc R . .
C10 C 0.0954(3) 0.26531(17) 0.4707(4) 0.0379(10) Uani 1 1 d . . .
H10A H 0.1245 0.2797 0.5644 0.057 Uiso 1 1 calc R . .
H10B H 0.0340 0.2903 0.4191 0.057 Uiso 1 1 calc R . .
H10C H 0.1446 0.2720 0.4329 0.057 Uiso 1 1 calc R . .
Al1 Al 0.5000 0.12688(7) 0.2500 0.0180(3) Uani 1 2 d S . .
Cl1 Cl 0.36810(6) 0.18497(4) 0.14731(8) 0.0237(2) Uani 1 1 d . . .
Cl2 Cl 0.52438(7) 0.06672(4) 0.10840(8) 0.0264(2) Uani 1 1 d . . .
Cl3 Cl 0.0000 0.0000 0.0000 0.0262(3) Uani 1 2 d S . .


_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
P1 C7 1.777(4) . ?
P1 C8 1.783(3) . ?
P1 C1 1.799(3) . ?
P1 H1 1.29(3) . ?
P2 C10 1.836(4) . ?
P2 C9 1.838(3) . ?
P2 C2 1.845(3) . ?
C1 C6 1.398(4) . ?
C1 C2 1.404(4) . ?
C2 C3 1.399(4) . ?
C3 C4 1.379(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.381(4) . ?
C4 H4 0.9500 . ?
C5 C6 1.385(4) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
Al1 Cl2 2.1383(13) . ?
Al1 Cl2 2.1383(13) 2_655 ?
Al1 Cl1 2.1410(12) 2_655 ?
Al1 Cl1 2.1410(12) . ?

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
C7 P1 C8 108.79(18) . . ?
C7 P1 C1 111.31(17) . . ?
C8 P1 C1 110.64(15) . . ?
C7 P1 H1 109.1(14) . . ?
C8 P1 H1 106.7(13) . . ?
C1 P1 H1 110.2(13) . . ?
C10 P2 C9 101.31(17) . . ?
C10 P2 C2 100.15(15) . . ?
C9 P2 C2 100.94(15) . . ?
C6 C1 C2 120.4(3) . . ?
C6 C1 P1 118.7(2) . . ?
C2 C1 P1 120.8(2) . . ?
C3 C2 C1 117.9(3) . . ?
C3 C2 P2 122.2(2) . . ?
C1 C2 P2 120.0(2) . . ?
C4 C3 C2 121.4(3) . . ?
C4 C3 H3 119.3 . . ?
C2 C3 H3 119.3 . . ?
C3 C4 C5 120.3(3) . . ?
C3 C4 H4 119.8 . . ?
C5 C4 H4 119.8 . . ?
C4 C5 C6 119.8(3) . . ?
C4 C5 H5 120.1 . . ?
C6 C5 H5 120.1 . . ?
C5 C6 C1 120.2(3) . . ?
C5 C6 H6 119.9 . . ?
C1 C6 H6 119.9 . . ?
P1 C7 H7A 109.5 . . ?
P1 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
P1 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
P1 C8 H8A 109.5 . . ?
P1 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
P1 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
P2 C9 H9A 109.5 . . ?
P2 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
P2 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
P2 C10 H10A 109.5 . . ?
P2 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
P2 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
Cl2 Al1 Cl2 108.87(8) . 2_655 ?
Cl2 Al1 Cl1 108.71(4) . 2_655 ?
Cl2 Al1 Cl1 109.37(4) 2_655 2_655 ?
Cl2 Al1 Cl1 109.37(4) . . ?
Cl2 Al1 Cl1 108.71(4) 2_655 . ?
Cl1 Al1 Cl1 111.76(8) 2_655 . ?

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
C7 P1 C1 C6 24.9(3) . . . . ?
C8 P1 C1 C6 -96.2(3) . . . . ?
C7 P1 C1 C2 -156.7(3) . . . . ?
C8 P1 C1 C2 82.2(3) . . . . ?
C6 C1 C2 C3 -1.6(5) . . . . ?
P1 C1 C2 C3 179.9(2) . . . . ?
C6 C1 C2 P2 178.0(2) . . . . ?
P1 C1 C2 P2 -0.4(4) . . . . ?
C10 P2 C2 C3 51.2(3) . . . . ?
C9 P2 C2 C3 -52.5(3) . . . . ?
C10 P2 C2 C1 -128.4(3) . . . . ?
C9 P2 C2 C1 127.9(3) . . . . ?
C1 C2 C3 C4 1.2(5) . . . . ?
P2 C2 C3 C4 -178.4(2) . . . . ?
C2 C3 C4 C5 0.0(5) . . . . ?
C3 C4 C5 C6 -0.8(5) . . . . ?
C4 C5 C6 C1 0.4(5) . . . . ?
C2 C1 C6 C5 0.8(5) . . . . ?
P1 C1 C6 C5 179.3(2) . . . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.358
_refine_diff_density_min         -0.361
_refine_diff_density_rms         0.085

_iucr_refine_instruction_details 
;
 Add final .res file here for Acta Cryst publications or if required.
;
_database_code_depnum_ccdc_archive 'CCDC 1005868'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_[Cy2HP(CH2)2PHCy2][AlCl4]2
#data_13jebr20 

_audit_creation_method           'SHELXL-97 + hand edit'
_audit_creation_date             2013-08-21 # yyyy-mm-dd


_chemical_name_systematic        
; 
 ethane-1,2-diylbis(dicyclohexylphosphonium) tetrachloroaluminate
;

# [(C6H11)2HPCH2CH2PH(C6H11)2]2+ = [C26H50P2]2+ = [Cy2HP(CH2)2PHCy2]2+
# ethane-1,2-diylbis(dicyclohexylphosphonium) (ACD I-Lab2) 

_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C26 H50 P2 2+, 2(Al Cl4 1-)'
_chemical_formula_sum            'C26 H50 Al2 Cl8 P2'
_chemical_formula_weight         762.16

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'
Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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_name_H-M_alt        'P 21/c'
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'


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

_cell_length_a                   7.073(6)
_cell_length_b                   17.551(13)
_cell_length_c                   14.924(13)
_cell_angle_alpha                90.00
_cell_angle_beta                 101.682(15)
_cell_angle_gamma                90.00
_cell_volume                     1814(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    4841
_cell_measurement_theta_min      2.9
_cell_measurement_theta_max      34.6

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.395
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             796
_exptl_absorpt_coefficient_mu    0.775
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.556 # Expt'l Tmin & Tmax
_exptl_absorpt_correction_T_max  1.000 # scaled to Tmax=1.0
_exptl_absorpt_process_details   
;Jacobson, R.A. (1998). REQAB. Private communication to the 
 Rigaku Corporation, Tokyo, Japan. 
;


_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  ?
_diffrn_radiation_collimation    'Confocal mirrors, VHF VariMax '

_diffrn_source                   'Rotating anode X-ray tube'
_diffrn_source_type              'Rigaku FR-E+ Superbright'

_diffrn_measurement_device       'Four-circle κ diffractometer'
_diffrn_measurement_device_type  'Rigaku AFC12 '
_diffrn_measurement_method       'Profile data from ω-scans'

_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Rigaku HG Saturn724+ (2x2 bin mode)'
_diffrn_detector_area_resol_mean ?

_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            10205
_diffrn_reflns_av_R_equivalents  0.0741
_diffrn_reflns_av_sigmaI/netI    0.0971
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.32
_diffrn_reflns_theta_max         26.00
_reflns_number_total             3545
_reflns_number_gt                2828
_reflns_threshold_expression     I>2σ(I)


_computing_data_collection       'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)'
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'ORTEP-III (Farrugia, 1997)'
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger.

 H1 bonded to P1 was clear as the Q2 peak in the difference map.
 It was added to the model with refined x,y,z and a fixed Uiso. 

 The largest differenc epeak is: 
 Q1 1 0.5570  0.5723  0.8840 1.00000 0.05 
 1.21 angstroms from P1
 Not in a chemically meaningful position.  
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0432P)²+3.9655P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed # constr (C-H) refxyz (P-H) 
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3545
_refine_ls_number_parameters     175
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1146
_refine_ls_R_factor_gt           0.0884
_refine_ls_wR_factor_ref         0.1786
_refine_ls_wR_factor_gt          0.1658
_refine_ls_goodness_of_fit_ref   1.183
_refine_ls_restrained_S_all      1.183
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
P1 P 0.4124(2) 0.59766(9) 0.90513(10) 0.0268(4) Uani 1 1 d . . .
H1 H 0.257(9) 0.612(3) 0.943(4) 0.035 Uiso 1 1 d . . .
C1 C 0.5871(9) 0.6717(3) 0.9462(4) 0.0257(13) Uani 1 1 d . . .
H1A H 0.6387 0.6622 1.0127 0.031 Uiso 1 1 calc R . .
C2 C 0.7589(9) 0.6709(3) 0.8976(4) 0.0279(13) Uani 1 1 d . . .
H2A H 0.8270 0.6215 0.9085 0.033 Uiso 1 1 calc R . .
H2B H 0.7115 0.6768 0.8308 0.033 Uiso 1 1 calc R . .
C3 C 0.8983(9) 0.7354(3) 0.9331(4) 0.0307(14) Uani 1 1 d . . .
H3A H 0.9563 0.7261 0.9983 0.037 Uiso 1 1 calc R . .
H3B H 1.0039 0.7359 0.8985 0.037 Uiso 1 1 calc R . .
C4 C 0.7992(10) 0.8122(3) 0.9238(4) 0.0345(15) Uani 1 1 d . . .
H4A H 0.7534 0.8241 0.8581 0.041 Uiso 1 1 calc R . .
H4B H 0.8929 0.8520 0.9506 0.041 Uiso 1 1 calc R . .
C5 C 0.6274(10) 0.8131(3) 0.9721(4) 0.0324(15) Uani 1 1 d . . .
H5A H 0.6750 0.8071 1.0388 0.039 Uiso 1 1 calc R . .
H5B H 0.5607 0.8629 0.9615 0.039 Uiso 1 1 calc R . .
C6 C 0.4849(9) 0.7495(3) 0.9374(4) 0.0283(13) Uani 1 1 d . . .
H6A H 0.4247 0.7590 0.8725 0.034 Uiso 1 1 calc R . .
H6B H 0.3813 0.7491 0.9732 0.034 Uiso 1 1 calc R . .
C7 C 0.3458(9) 0.5984(3) 0.7807(3) 0.0275(14) Uani 1 1 d . . .
H7 H 0.3667 0.6517 0.7611 0.033 Uiso 1 1 calc R . .
C8 C 0.1342(10) 0.5807(4) 0.7445(4) 0.0349(15) Uani 1 1 d . . .
H8A H 0.0537 0.6165 0.7719 0.042 Uiso 1 1 calc R . .
H8B H 0.1059 0.5284 0.7629 0.042 Uiso 1 1 calc R . .
C9 C 0.0824(10) 0.5873(4) 0.6401(4) 0.0368(16) Uani 1 1 d . . .
H9A H -0.0536 0.5716 0.6184 0.044 Uiso 1 1 calc R . .
H9B H 0.0944 0.6411 0.6224 0.044 Uiso 1 1 calc R . .
C10 C 0.2108(11) 0.5386(4) 0.5946(4) 0.0394(17) Uani 1 1 d . . .
H10A H 0.1790 0.5477 0.5277 0.047 Uiso 1 1 calc R . .
H10B H 0.1855 0.4842 0.6053 0.047 Uiso 1 1 calc R . .
C11 C 0.4231(10) 0.5554(4) 0.6302(4) 0.0398(17) Uani 1 1 d . . .
H11A H 0.4521 0.6079 0.6131 0.048 Uiso 1 1 calc R . .
H11B H 0.5022 0.5199 0.6016 0.048 Uiso 1 1 calc R . .
C12 C 0.4771(10) 0.5468(4) 0.7352(4) 0.0363(15) Uani 1 1 d . . .
H12A H 0.6139 0.5612 0.7572 0.044 Uiso 1 1 calc R . .
H12B H 0.4614 0.4930 0.7522 0.044 Uiso 1 1 calc R . .
C13 C 0.4916(9) 0.5040(3) 0.9480(3) 0.0283(14) Uani 1 1 d . . .
H13A H 0.3992 0.4655 0.9166 0.034 Uiso 1 1 calc R . .
H13B H 0.6189 0.4932 0.9329 0.034 Uiso 1 1 calc R . .
Al1 Al 0.1270(3) 0.85864(10) 0.69738(11) 0.0272(4) Uani 1 1 d . . .
Cl1 Cl 0.1904(2) 0.91086(9) 0.82862(9) 0.0332(4) Uani 1 1 d . . .
Cl2 Cl 0.0179(2) 0.94205(8) 0.59351(9) 0.0330(4) Uani 1 1 d . . .
Cl3 Cl -0.0870(3) 0.77338(9) 0.69547(10) 0.0400(4) Uani 1 1 d . . .
Cl4 Cl 0.3834(3) 0.81158(10) 0.66380(10) 0.0417(5) 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
P1 C13 1.811(6) . ?
P1 C1 1.812(6) . ?
P1 C7 1.822(6) . ?
P1 H1 1.36(6) . ?
C1 C2 1.536(8) . ?
C1 C6 1.539(8) . ?
C1 H1A 1.0000 . ?
C2 C3 1.524(8) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.512(8) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 C5 1.534(9) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C6 1.523(8) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C8 1.517(9) . ?
C7 C12 1.549(8) . ?
C7 H7 1.0000 . ?
C8 C9 1.531(8) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C10 1.506(9) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 C11 1.517(10) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C12 1.542(8) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 C13 1.538(10) 3_667 ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
Al1 Cl3 2.124(3) . ?
Al1 Cl1 2.126(3) . ?
Al1 Cl4 2.143(3) . ?
Al1 Cl2 2.158(3) . ?

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
C13 P1 C1 113.0(3) . . ?
C13 P1 C7 111.4(3) . . ?
C1 P1 C7 111.0(3) . . ?
C13 P1 H1 104(2) . . ?
C1 P1 H1 106(2) . . ?
C7 P1 H1 111(2) . . ?
C2 C1 C6 111.7(4) . . ?
C2 C1 P1 112.6(4) . . ?
C6 C1 P1 109.3(4) . . ?
C2 C1 H1A 107.6 . . ?
C6 C1 H1A 107.6 . . ?
P1 C1 H1A 107.6 . . ?
C3 C2 C1 110.4(5) . . ?
C3 C2 H2A 109.6 . . ?
C1 C2 H2A 109.6 . . ?
C3 C2 H2B 109.6 . . ?
C1 C2 H2B 109.6 . . ?
H2A C2 H2B 108.1 . . ?
C4 C3 C2 112.0(5) . . ?
C4 C3 H3A 109.2 . . ?
C2 C3 H3A 109.2 . . ?
C4 C3 H3B 109.2 . . ?
C2 C3 H3B 109.2 . . ?
H3A C3 H3B 107.9 . . ?
C3 C4 C5 111.3(5) . . ?
C3 C4 H4A 109.4 . . ?
C5 C4 H4A 109.4 . . ?
C3 C4 H4B 109.4 . . ?
C5 C4 H4B 109.4 . . ?
H4A C4 H4B 108.0 . . ?
C6 C5 C4 111.4(5) . . ?
C6 C5 H5A 109.3 . . ?
C4 C5 H5A 109.3 . . ?
C6 C5 H5B 109.3 . . ?
C4 C5 H5B 109.3 . . ?
H5A C5 H5B 108.0 . . ?
C5 C6 C1 110.8(5) . . ?
C5 C6 H6A 109.5 . . ?
C1 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
C1 C6 H6B 109.5 . . ?
H6A C6 H6B 108.1 . . ?
C8 C7 C12 111.1(5) . . ?
C8 C7 P1 113.2(4) . . ?
C12 C7 P1 112.9(4) . . ?
C8 C7 H7 106.4 . . ?
C12 C7 H7 106.4 . . ?
P1 C7 H7 106.4 . . ?
C7 C8 C9 111.2(5) . . ?
C7 C8 H8A 109.4 . . ?
C9 C8 H8A 109.4 . . ?
C7 C8 H8B 109.4 . . ?
C9 C8 H8B 109.4 . . ?
H8A C8 H8B 108.0 . . ?
C10 C9 C8 112.0(5) . . ?
C10 C9 H9A 109.2 . . ?
C8 C9 H9A 109.2 . . ?
C10 C9 H9B 109.2 . . ?
C8 C9 H9B 109.2 . . ?
H9A C9 H9B 107.9 . . ?
C9 C10 C11 112.1(5) . . ?
C9 C10 H10A 109.2 . . ?
C11 C10 H10A 109.2 . . ?
C9 C10 H10B 109.2 . . ?
C11 C10 H10B 109.2 . . ?
H10A C10 H10B 107.9 . . ?
C10 C11 C12 111.2(5) . . ?
C10 C11 H11A 109.4 . . ?
C12 C11 H11A 109.4 . . ?
C10 C11 H11B 109.4 . . ?
C12 C11 H11B 109.4 . . ?
H11A C11 H11B 108.0 . . ?
C11 C12 C7 109.9(5) . . ?
C11 C12 H12A 109.7 . . ?
C7 C12 H12A 109.7 . . ?
C11 C12 H12B 109.7 . . ?
C7 C12 H12B 109.7 . . ?
H12A C12 H12B 108.2 . . ?
C13 C13 P1 113.3(5) 3_667 . ?
C13 C13 H13A 108.9 3_667 . ?
P1 C13 H13A 108.9 . . ?
C13 C13 H13B 108.9 3_667 . ?
P1 C13 H13B 108.9 . . ?
H13A C13 H13B 107.7 . . ?
Cl3 Al1 Cl1 109.44(10) . . ?
Cl3 Al1 Cl4 111.08(12) . . ?
Cl1 Al1 Cl4 110.54(11) . . ?
Cl3 Al1 Cl2 108.56(11) . . ?
Cl1 Al1 Cl2 110.32(11) . . ?
Cl4 Al1 Cl2 106.85(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
C13 P1 C1 C2 75.8(4) . . . . ?
C7 P1 C1 C2 -50.1(5) . . . . ?
C13 P1 C1 C6 -159.3(4) . . . . ?
C7 P1 C1 C6 74.8(4) . . . . ?
C6 C1 C2 C3 55.0(6) . . . . ?
P1 C1 C2 C3 178.6(4) . . . . ?
C1 C2 C3 C4 -55.6(6) . . . . ?
C2 C3 C4 C5 56.0(6) . . . . ?
C3 C4 C5 C6 -55.4(6) . . . . ?
C4 C5 C6 C1 54.7(6) . . . . ?
C2 C1 C6 C5 -55.1(6) . . . . ?
P1 C1 C6 C5 179.5(4) . . . . ?
C13 P1 C7 C8 90.6(5) . . . . ?
C1 P1 C7 C8 -142.7(4) . . . . ?
C13 P1 C7 C12 -36.8(5) . . . . ?
C1 P1 C7 C12 90.0(5) . . . . ?
C12 C7 C8 C9 -55.6(7) . . . . ?
P1 C7 C8 C9 176.1(4) . . . . ?
C7 C8 C9 C10 54.6(7) . . . . ?
C8 C9 C10 C11 -54.5(7) . . . . ?
C9 C10 C11 C12 55.4(7) . . . . ?
C10 C11 C12 C7 -55.7(7) . . . . ?
C8 C7 C12 C11 56.3(7) . . . . ?
P1 C7 C12 C11 -175.3(4) . . . . ?
C1 P1 C13 C13 66.5(7) . . . 3_667 ?
C7 P1 C13 C13 -167.8(6) . . . 3_667 ?

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         1.025
_refine_diff_density_min         -0.458
_refine_diff_density_rms         0.101

_iucr_refine_instruction_details 
;
 Add final .res file here for Acta Cryst publications or if required.
;
_database_code_depnum_ccdc_archive 'CCDC 1005869'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_[o-C6H4(PMe2)(PHMe2)]2[AlBr4][Br]
#data_jebx

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C10 H17 P2 1+), Al Br4 1-, Br 1-'
_chemical_formula_sum            'C20 H34 Al Br5 P4'
_chemical_formula_weight         824.88

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'
Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_name_H-M_alt        'C 2/c'
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'

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

_cell_length_a                   14.834(7)
_cell_length_b                   21.144(8)
_cell_length_c                   11.274(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 115.646(6)
_cell_angle_gamma                90.00
_cell_volume                     3188(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    3917
_cell_measurement_theta_min      2.1
_cell_measurement_theta_max      27.5

_exptl_crystal_description       platelet
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.719
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1608
_exptl_absorpt_coefficient_mu    6.540
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6574
_exptl_absorpt_correction_T_max  0.6950
_exptl_absorpt_process_details   'CrystalClear-SM Expert 2.0 r11 (Rigaku, 2011)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source_power             2.5
_diffrn_source_voltage           45.0
_diffrn_source_current           55.0
_diffrn_source                   'Rotating Anode'
_diffrn_radiation_monochromator  Confocal
_diffrn_measurement_specimen_support Mitegen
_diffrn_detector                 CCD
_diffrn_measurement_device       
;
AFC12 (Right): Kappa 3 circle
;
_diffrn_measurement_device_type  
;
Rigaku Saturn724+ (2x2 bin mode)
;
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            13640
_diffrn_reflns_av_R_equivalents  0.0306
_diffrn_reflns_av_sigmaI/netI    0.0353
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         3.05
_diffrn_reflns_theta_max         27.46
_reflns_number_total             3631
_reflns_number_gt                3260
_reflns_threshold_expression     >2σ(I)

_computing_data_collection       
;
CrystalClear-SM Expert 2.0 r11 (Rigaku, 2011)
;
_computing_cell_refinement       
;
CrystalClear-SM Expert 2.0 r11 (Rigaku, 2011)
;
_computing_data_reduction        
;
CrystalClear-SM Expert 2.0 r11 (Rigaku, 2011)
;
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0231P)²+0.4756P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3631
_refine_ls_number_parameters     146
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0382
_refine_ls_R_factor_gt           0.0321
_refine_ls_wR_factor_ref         0.0551
_refine_ls_wR_factor_gt          0.0532
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_restrained_S_all      1.071
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C7 C 0.3122(2) 0.38971(13) 0.2440(3) 0.0271(6) Uani 1 1 d . . .
H7A H 0.3462 0.4084 0.3319 0.041 Uiso 1 1 calc R . .
H7B H 0.3390 0.3473 0.2444 0.041 Uiso 1 1 calc R . .
H7C H 0.2404 0.3868 0.2192 0.041 Uiso 1 1 calc R . .
C8 C 0.2893(2) 0.51654(14) 0.1337(3) 0.0352(7) Uani 1 1 d . . .
H8A H 0.2180 0.5153 0.1133 0.053 Uiso 1 1 calc R . .
H8B H 0.2991 0.5430 0.0689 0.053 Uiso 1 1 calc R . .
H8C H 0.3271 0.5342 0.2219 0.053 Uiso 1 1 calc R . .
C9 C 0.4017(2) 0.23794(14) 0.0316(3) 0.0419(8) Uani 1 1 d . . .
H9A H 0.3720 0.2239 -0.0603 0.063 Uiso 1 1 calc R . .
H9B H 0.3537 0.2316 0.0688 0.063 Uiso 1 1 calc R . .
H9C H 0.4624 0.2134 0.0821 0.063 Uiso 1 1 calc R . .
C10 C 0.5015(2) 0.32375(14) -0.0635(3) 0.0320(7) Uani 1 1 d . . .
H10A H 0.5661 0.3025 -0.0171 0.048 Uiso 1 1 calc R . .
H10B H 0.5125 0.3676 -0.0820 0.048 Uiso 1 1 calc R . .
H10C H 0.4620 0.3017 -0.1464 0.048 Uiso 1 1 calc R . .
H1 H 0.4243(19) 0.4407(12) 0.157(2) 0.023(7) Uiso 1 1 d . . .
C1 C 0.26886(18) 0.40580(12) -0.0356(2) 0.0168(5) Uani 1 1 d . . .
C2 C 0.31178(19) 0.35565(12) -0.0751(2) 0.0191(6) Uani 1 1 d . . .
C3 C 0.25878(19) 0.33199(13) -0.2029(2) 0.0224(6) Uani 1 1 d . . .
H3 H 0.2865 0.2985 -0.2327 0.027 Uiso 1 1 calc R . .
C4 C 0.1662(2) 0.35692(13) -0.2866(3) 0.0244(6) Uani 1 1 d . . .
H4 H 0.1311 0.3402 -0.3728 0.029 Uiso 1 1 calc R . .
C5 C 0.1249(2) 0.40561(13) -0.2458(3) 0.0236(6) Uani 1 1 d . . .
H5 H 0.0615 0.4222 -0.3034 0.028 Uiso 1 1 calc R . .
C6 C 0.1761(2) 0.43042(13) -0.1206(3) 0.0225(6) Uani 1 1 d . . .
H6 H 0.1478 0.4643 -0.0925 0.027 Uiso 1 1 calc R . .
Al1 Al 0.0000 0.36742(5) -0.7500 0.0162(2) Uani 1 2 d S . .
P1 P 0.33233(5) 0.43825(3) 0.12808(7) 0.02107(16) Uani 1 1 d . . .
P2 P 0.43395(5) 0.32269(4) 0.03933(7) 0.02629(17) Uani 1 1 d . . .
Br1 Br 0.140908(19) 0.307558(12) -0.63665(2) 0.02121(8) Uani 1 1 d . . .
Br2 Br -0.02692(2) 0.431065(13) -0.60321(3) 0.02409(8) Uani 1 1 d . . .
Br3 Br 0.5000 0.5000 0.0000 0.02734(10) Uani 1 2 d S . .


_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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
C7 P1 1.785(3) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 P1 1.785(3) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 P2 1.847(3) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 P2 1.831(3) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C1 C6 1.394(4) . ?
C1 C2 1.405(3) . ?
C1 P1 1.805(3) . ?
C2 C3 1.401(4) . ?
C2 P2 1.847(3) . ?
C3 C4 1.390(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.375(4) . ?
C4 H4 0.9500 . ?
C5 C6 1.384(4) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
Al1 Br2 2.2981(9) . ?
Al1 Br2 2.2981(9) 2_553 ?
Al1 Br1 2.3004(9) 2_553 ?
Al1 Br1 2.3004(9) . ?
P1 H1 1.26(3) . ?

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
P1 C7 H7A 109.5 . . ?
P1 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
P1 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
P1 C8 H8A 109.5 . . ?
P1 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
P1 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
P2 C9 H9A 109.5 . . ?
P2 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
P2 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
P2 C10 H10A 109.5 . . ?
P2 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
P2 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C6 C1 C2 120.8(2) . . ?
C6 C1 P1 118.9(2) . . ?
C2 C1 P1 120.3(2) . . ?
C3 C2 C1 117.8(2) . . ?
C3 C2 P2 121.9(2) . . ?
C1 C2 P2 120.3(2) . . ?
C4 C3 C2 120.8(2) . . ?
C4 C3 H3 119.6 . . ?
C2 C3 H3 119.6 . . ?
C5 C4 C3 120.6(3) . . ?
C5 C4 H4 119.7 . . ?
C3 C4 H4 119.7 . . ?
C4 C5 C6 119.9(3) . . ?
C4 C5 H5 120.1 . . ?
C6 C5 H5 120.1 . . ?
C5 C6 C1 120.1(3) . . ?
C5 C6 H6 119.9 . . ?
C1 C6 H6 119.9 . . ?
Br2 Al1 Br2 108.31(5) . 2_553 ?
Br2 Al1 Br1 108.84(3) . 2_553 ?
Br2 Al1 Br1 108.75(3) 2_553 2_553 ?
Br2 Al1 Br1 108.75(3) . . ?
Br2 Al1 Br1 108.84(3) 2_553 . ?
Br1 Al1 Br1 113.24(5) 2_553 . ?
C7 P1 C8 109.36(14) . . ?
C7 P1 C1 110.56(13) . . ?
C8 P1 C1 110.63(14) . . ?
C7 P1 H1 109.7(11) . . ?
C8 P1 H1 108.5(11) . . ?
C1 P1 H1 108.1(11) . . ?
C10 P2 C9 100.55(14) . . ?
C10 P2 C2 101.13(13) . . ?
C9 P2 C2 100.23(13) . . ?

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
C6 C1 C2 C3 0.8(4) . . . . ?
P1 C1 C2 C3 179.46(19) . . . . ?
C6 C1 C2 P2 -179.10(19) . . . . ?
P1 C1 C2 P2 -0.4(3) . . . . ?
C1 C2 C3 C4 -0.9(4) . . . . ?
P2 C2 C3 C4 179.0(2) . . . . ?
C2 C3 C4 C5 0.3(4) . . . . ?
C3 C4 C5 C6 0.4(4) . . . . ?
C4 C5 C6 C1 -0.5(4) . . . . ?
C2 C1 C6 C5 -0.1(4) . . . . ?
P1 C1 C6 C5 -178.8(2) . . . . ?
C6 C1 P1 C7 98.4(2) . . . . ?
C2 C1 P1 C7 -80.3(2) . . . . ?
C6 C1 P1 C8 -22.9(2) . . . . ?
C2 C1 P1 C8 158.4(2) . . . . ?
C3 C2 P2 C10 50.4(2) . . . . ?
C1 C2 P2 C10 -129.7(2) . . . . ?
C3 C2 P2 C9 -52.6(2) . . . . ?
C1 C2 P2 C9 127.3(2) . . . . ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        27.46
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         0.557
_refine_diff_density_min         -0.378
_refine_diff_density_rms         0.096



#===END 


_database_code_depnum_ccdc_archive 'CCDC 1005870'
