New Synthetic and Structural Aspects in the Chemistry of Alkylaluminum Fluorides. The Mutual Influence of Hard and Soft Ligands and the Hybridization as Rigorous Structural Criterion#
Marilena Ferbinteanu; Herbert W. Roesky; Fanica Cimpoesu; Mihail Atanasov; Sinje Köpke; Regine Herbst-Irmer; Inorganic Chemistry 40 (2001) 4947–4955; doi:10.1021/ic010131g

data_4320244
_publ_contact_author
;
     Dr. Regine Herbst-Irmer
     Institut f\"ur Anorganische Chemie
     Universit\"at G\"ottingen
     Tammannstr. 4
     37077 G\"ottingen
     Germany
;
_publ_contact_author_email       rherbst@shelx.uni-ac.gwdg.de
_publ_contact_author_fax         '049 551 392582'
_publ_contact_author_phone       '049 551 393007'
_publ_section_title
;
 New Synthetic and Structural Aspects in the Chemistry of Alkylaluminum
 Fluorides. The Mutual Influence of Hard and Soft Ligands and the
 Hybridization as Rigorous Structural Criterion#
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4947
_journal_page_last               4955
_journal_paper_doi               10.1021/ic010131g
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C12 H30 Al F2 N'
_chemical_formula_weight         253.35
_chemical_name_systematic
;
?
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.208(4)
_cell_length_b                   8.783(2)
_cell_length_c                   9.720(2)
_cell_measurement_reflns_used    1012
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      27.67
_cell_measurement_theta_min      2.35
_cell_volume                     1639.8(6)
_computing_cell_refinement       'Siemens SAINT (V. 6.08b, BRUKER 1999)'
_computing_data_collection       'Siemens SMART (V.5.050, Siemens 1998)'
_computing_data_reduction        'Siemens SAINT (V. 6.08b, BRUKER 1999)'
_computing_molecular_graphics    'Bruker AXS SHELXTL (V. 5.10)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      133(2)
_diffrn_detector_area_resol_mean '8.192 pixels/mm'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type
'STOE-Siemens-Huber four circle diffractometer'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0364
_diffrn_reflns_av_sigmaI/netI    0.0197
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            68853
_diffrn_reflns_theta_full        27.67
_diffrn_reflns_theta_max         27.67
_diffrn_reflns_theta_min         2.35
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.124
_exptl_absorpt_correction_T_max  0.9756
_exptl_absorpt_correction_T_min  0.9521
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.026
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             560
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.615
_refine_diff_density_min         -0.388
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.147
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     109
_refine_ls_number_reflns         2033
_refine_ls_number_restraints     62
_refine_ls_restrained_S_all      1.142
_refine_ls_R_factor_all          0.0744
_refine_ls_R_factor_gt           0.0696
_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^)+(0.0811P)^2^+1.1400P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1816
_refine_ls_wR_factor_ref         0.1860
_reflns_number_gt                1882
_reflns_number_total             2033
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic010131g_2.cif
_cod_data_source_block           misch
_cod_database_code               4320244