Redetermination of an acyclic triphosphenium tetrachloroaluminate salt at 173K
Ellis, Bobby D.; Macdonald, Charles L. B.; Acta Crystallographica Section E 62 (2006) m1869–m1870; doi:10.1107/S160053680602722X

data_2209946
_publ_section_title
;
 Redetermination of an acyclic triphosphenium tetrachloroaluminate salt
 at 173K
;
_journal_coeditor_code           LH2136
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1869
_journal_page_last               m1870
_journal_paper_doi               10.1107/S160053680602722X
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          '(C36 H30 P3) [Al Cl4], 0.5C H2 Cl2'
_chemical_formula_moiety         'C36 H30 P3 +, Cl4 Al -, 0.5C H2 Cl2'
_chemical_formula_sum            'C73 H62 Al2 Cl10 P6'
_chemical_formula_weight         766.76
_chemical_melting_point          78
_chemical_name_common
;
[(Ph3P)2P +] [AlCl4 -] . 0.5 CH2Cl2
;
_chemical_name_systematic
;
1,1,1,3,3,3-hexaphenyltriphosphenium tetrachloroaluminate dichloromethane
hemisolvate
;
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   33.283(5)
_cell_length_b                   9.2443(13)
_cell_length_c                   23.979(4)
_cell_measurement_reflns_used    7634
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      1.22
_cell_volume                     7378(2)
_computing_cell_refinement       'SAINT-Plus (Bruker, 1997)'
_computing_data_collection       'SMART (Bruker, 1997)'
_computing_data_reduction        SAINT-Plus
_computing_molecular_graphics    'SHELXTL (Bruker, 1997)'
_computing_publication_material
'SHELXTL, PLATON (Spek, 2003) and WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0428
_diffrn_reflns_av_sigmaI/netI    0.0398
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            79631
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.22
_exptl_absorpt_coefficient_mu    0.573
_exptl_absorpt_correction_T_max  0.795
_exptl_absorpt_correction_T_min  0.652
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2000)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.381
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3144
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.40
_refine_diff_density_max         1.563
_refine_diff_density_min         -0.615
_refine_ls_abs_structure_details 'Flack (1983), 8081 Friedel pairs'
_refine_ls_abs_structure_Flack   -0.01(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     821
_refine_ls_number_reflns         16737
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0633
_refine_ls_R_factor_gt           0.0492
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0795P)^2^+1.5731P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1176
_refine_ls_wR_factor_ref         0.1310
_reflns_number_gt                14199
_reflns_number_total             16737
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            lh2136.cif
_cod_data_source_block           I
_cod_database_code               2209946
_cod_database_fobs_code          2209946