#------------------------------------------------------------------------------
#$Date: 2023-12-22 17:07:40 +0200 (Fri, 22 Dec 2023) $
#$Revision: 288505 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/03/19/7031947.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7031947
loop_
_publ_author_name
'Burt, Jennifer'
'Levason, William'
'Light, Mark E.'
'Reid, Gillian'
_publ_section_title
;
 Phosphine complexes of aluminium(iii) halides - preparation and
 structural and spectroscopic systematics.
;
_journal_issue                   39
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14600
_journal_page_last               14611
_journal_paper_doi               10.1039/c4dt02051k
_journal_volume                  43
_journal_year                    2014
_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
_chemical_name_systematic
; 
 dichlorobis(1,2-bis(dimethylphosphino)benzene)aluminium(III)
 tetrachloroaluminate  
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-08-15
_audit_creation_method           'SHELXL-97 + hand edit'
_cell_angle_alpha                90.00
_cell_angle_beta                 104.126(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.278(4)
_cell_length_b                   14.545(4)
_cell_length_c                   16.554(5)
_cell_measurement_reflns_used    5045
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      34.9
_cell_measurement_theta_min      2.1
_cell_volume                     3100.4(16)
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)'
_computing_data_collection       'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)'
_computing_molecular_graphics    'ORTEP-III (Farrugia, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Rigaku HG Saturn724+ (2x2 bin mode)'
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       'Four-circle κ diffractometer'
_diffrn_measurement_device_type  'Rigaku AFC12 '
_diffrn_measurement_method       'Profile data from ω-scans'
_diffrn_radiation_collimation    'Confocal mirrors, VHF VariMax '
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0321
_diffrn_reflns_av_unetI/netI     0.0301
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            14366
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         3.59
_diffrn_source                   'Rotating anode X-ray tube'
_diffrn_source_type              'Rigaku FR-E+ Superbright'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.828
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.902
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;Jacobson, R.A. (1998). REQAB. Private communication to the 
 Rigaku Corporation, Tokyo, Japan. 
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.420
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1360
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.419
_refine_diff_density_min         -0.226
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     151
_refine_ls_number_reflns         3544
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0352
_refine_ls_R_factor_gt           0.0300
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0273P)²+2.1045P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0648
_refine_ls_wR_factor_ref         0.0671
_reflns_number_gt                3257
_reflns_number_total             3544
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            c4dt02051k2.cif
_cod_data_source_block           '[AlCl2{o-C6H4(PMe2)2}2][AlCl4]'
_cod_depositor_comments
;Adding full bibliography for 7031945--7031955.cif.

The following automatic conversions were performed:

data name '_iucr_refine_instruction_details' was replaced with
'_iucr_refine_instructions_details' as specified in the replacement
file 'data/replacement-values/replacement_tags.lst'.

Automatic conversion script
Id: cif_correct_tags 9268 2022-04-12 08:56:07Z antanas 
;
_cod_original_cell_volume        3100.2(16)
_cod_database_code               7031947
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'
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
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
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'
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
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_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
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_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
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)
