Phosphine complexes of aluminium(iii) halides - preparation and structural and spectroscopic systematics.
Burt, Jennifer; Levason, William; Light, Mark E.; Reid, Gillian; Dalton transactions (Cambridge, England : 2003) 43 (2014) 14600–14611; doi:10.1039/c4dt02051k

data_7031948
_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         'C60 H48 Al Cl2 P4 1+, Al Cl4 1-'
_chemical_formula_structural     '((C30 H24 P2)2 Al Cl2) (Al Cl4)'
_chemical_formula_sum            'C60 H48 Al2 Cl6 P4'
_chemical_formula_weight         1159.52
_chemical_name_systematic
; 
 bis(benzene-1,2-diylbis(diphenylphosphane))dichloroaluminium(III)
 tetrachloroaluminate 
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-09-11
_audit_creation_method           'SHELXL-97 + hand edit'
_cell_angle_alpha                81.926(14)
_cell_angle_beta                 85.52(2)
_cell_angle_gamma                82.25(2)
_cell_formula_units_Z            2
_cell_length_a                   10.024(3)
_cell_length_b                   11.752(4)
_cell_length_c                   24.434(8)
_cell_measurement_reflns_used    7440
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      34.6
_cell_measurement_theta_min      2.1
_cell_volume                     2818.7(16)
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r13 (Rigaku, 2011)'
_computing_data_collection       'CrystalClear-SM Expert 2.0 r13 (Rigaku, 2011)'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 r13 (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 0.943
_diffrn_measured_fraction_theta_max 0.943
_diffrn_measurement_device       'Four-circle \k diffractometer'
_diffrn_measurement_device_type  'Rigaku AFC12 '
_diffrn_measurement_method       'Profile data from \w-scans'
_diffrn_radiation_collimation    'Confocal mirrors, VHF VariMax '
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0757
_diffrn_reflns_av_unetI/netI     0.1460
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            24430
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.96
_diffrn_source                   'Rotating anode X-ray tube'
_diffrn_source_type              'Rigaku FR-E+ Superbright'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.489
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.817
_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    1.366
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1192
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.554
_refine_diff_density_min         -0.484
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     652
_refine_ls_number_reflns         12194
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.1354
_refine_ls_R_factor_gt           0.0793
_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/[\s^2^(Fo^2^)+(0.0595P)^2^+0.5098P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1594
_refine_ls_wR_factor_ref         0.1934
_reflns_number_gt                7266
_reflns_number_total             12194
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c4dt02051k2.cif
_cod_data_source_block           '[AlCl2{o-C6H4(PPh2)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        2818.9(16)
_cod_database_code               7031948