Syntheses and Characterization of Salts with the [Al(D)4F2]+ Cation (D = Pyridine or Water)
Anton Dimitrov; Detlef Heidemann; Khalaf I. Khallow; Erhard Kemnitz; Inorganic Chemistry 51 (2012) 11612–11622; doi:10.1021/ic301502u

data_4330852
_publ_contact_author
;
      Prof. Dr. Erhard Kemnitz
      Institut f\"ur Chemie
      Humboldt-Universit\"at zu Berlin
      Brook-Taylor Str.2
      12489 Berlin, 
      Germany
;
_publ_contact_author_email       erhard.kemnitz@chemie.hu-berlin.de
_publ_contact_author_fax         '+49 30 20937277'
_publ_contact_author_phone       '+49 30 20937555'
_publ_section_title
;
 Syntheses and Characterization of Salts with the [Al(D)4F2]+ Cation (D =
 Pyridine or Water)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11612
_journal_page_last               11622
_journal_paper_doi               10.1021/ic301502u
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         'Al F2 H8 O4, 2(C5 H6 N), 3(Cl)'
_chemical_formula_sum            'C10 H20 Al Cl3 F2 N2 O4'
_chemical_formula_weight         403.61
_chemical_name_systematic
; 
 trans-Difluoro-tetrakis(aqua)-aluminium bis(pyridinium) trichloride 
;
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 103.089(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   5.0967(3)
_cell_length_b                   19.7672(11)
_cell_length_c                   9.0423(7)
_cell_measurement_reflns_used    2543
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      59.53
_cell_measurement_theta_min      2.29
_cell_volume                     887.32(10)
_computing_cell_refinement       'X-AREA (Stoe & Cie, 2002)'
_computing_data_collection       'X-AREA (Stoe & Cie, 2002)'
_computing_data_reduction        'X-RED (Stoe & Cie, 2002)'
_computing_molecular_graphics    'PLATON, 1990'
_computing_publication_material  'PLATON, 1990'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'Stoe IPDS-2t diffractometer'
_diffrn_measurement_method       '\w-rotation,\w-incr.=1\%,319 exposures'
_diffrn_radiation_collimation    '0.5 mm diameter monocapillary'
_diffrn_radiation_monochromator  'planar graphite'
_diffrn_radiation_source         'long fine focus sealed x-ray tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0996
_diffrn_reflns_av_sigmaI/netI    0.0431
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            18004
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.31
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.600
_exptl_absorpt_correction_T_max  0.9480
_exptl_absorpt_correction_T_min  0.8894
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'PLATON, 1990'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.511
_exptl_crystal_description       plate
_exptl_crystal_F_000             416
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.314
_refine_diff_density_min         -0.338
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     170
_refine_ls_number_reflns         2105
_refine_ls_number_restraints     45
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0507
_refine_ls_R_factor_gt           0.0388
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0359P)^2^+0.2339P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0774
_refine_ls_wR_factor_ref         0.0810
_reflns_number_gt                1799
_reflns_number_total             2105
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic301502u_si_001_1.cif
_cod_data_source_block           V4
_cod_database_code               4330852