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_4330853
_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         'C20 H20 Al F2 N4, Br'
_chemical_formula_sum            'C20 H20 Al Br F2 N4'
_chemical_formula_weight         461.29
_chemical_name_common
; 
  trans-Difluoro-tetrakis(pyridine)-aluminium bromide 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_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_method           SHELXL-97
_audit_update_record
;
2012-07-13 # Formatted by publCIF
;
_cell_angle_alpha                90.00
_cell_angle_beta                 118.869(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.8509(5)
_cell_length_b                   11.8375(4)
_cell_length_c                   12.9196(4)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      50
_cell_measurement_theta_min      5
_cell_volume                     1988.98(12)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        XPREP
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_collimation    '0.5 mm diameter, monocapillary'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0583
_diffrn_reflns_av_sigmaI/netI    0.0265
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            15503
_diffrn_reflns_theta_full        29.13
_diffrn_reflns_theta_max         29.13
_diffrn_reflns_theta_min         2.33
_diffrn_source
'sealed x-ray tube, 12 x 0.4 mm long-fine focus'
_diffrn_source_current           45
_diffrn_source_power             2.25
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    2.142
_exptl_absorpt_correction_T_max  0.86593
_exptl_absorpt_correction_T_min  0.55005
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   PLATON
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.540
_exptl_crystal_description       block
_exptl_crystal_F_000             936
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.397
_refine_diff_density_min         -0.373
_refine_diff_density_rms         0.066
_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     129
_refine_ls_number_reflns         2678
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0401
_refine_ls_R_factor_gt           0.0322
_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^)+(0.0337P)^2^+1.1657P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0640
_refine_ls_wR_factor_ref         0.0660
_reflns_number_gt                2348
_reflns_number_total             2678
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic301502u_si_001_2.cif
_cod_data_source_block           2vb
_cod_original_cell_volume        1988.98(11)
_cod_database_code               4330853