Al/P-Based Frustrated Lewis Pairs: Limitations of Their Synthesis by Hydroalumination and Formation of Dialkylaluminum Hydride Adducts
Uhl, Werner; Appelt, Christian; Backs, Jana; Westenberg, Hauke; Wollschläger, Agnes; Tannert, Jens; Organometallics 33 (2014) 1212–; doi:10.1021/om4012246

data_4082651
_publ_section_title
;
 Al/P-Based Frustrated Lewis Pairs: Limitations of Their Synthesis by
 Hydroalumination and Formation of Dialkylaluminum Hydride Adducts
;
_journal_issue                   5
_journal_name_full               Organometallics
_journal_page_first              1212
_journal_paper_doi               10.1021/om4012246
_journal_volume                  33
_journal_year                    2014
_chemical_formula_sum            'C40 H61 Al2 P'
_chemical_formula_weight         626.82
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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_method           SHELXL-97
_cell_angle_alpha                110.5730(10)
_cell_angle_beta                 102.2030(10)
_cell_angle_gamma                94.3930(10)
_cell_formula_units_Z            4
_cell_length_a                   11.3168(2)
_cell_length_b                   17.7183(3)
_cell_length_c                   22.2271(3)
_cell_measurement_reflns_used    6317
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      72.50
_cell_measurement_theta_min      2.77
_cell_volume                     4022.52(12)
_computing_cell_refinement       'Bruker SAINT+'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.908
_diffrn_measured_fraction_theta_max 0.908
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0242
_diffrn_reflns_av_sigmaI/netI    0.0307
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            22962
_diffrn_reflns_theta_full        65.99
_diffrn_reflns_theta_max         65.99
_diffrn_reflns_theta_min         2.20
_exptl_absorpt_coefficient_mu    1.189
_exptl_absorpt_correction_T_max  0.9005
_exptl_absorpt_correction_T_min  0.7474
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.035
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1368
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.881
_refine_diff_density_min         -1.073
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1003
_refine_ls_number_reflns         12712
_refine_ls_number_restraints     1088
_refine_ls_restrained_S_all      1.112
_refine_ls_R_factor_all          0.0624
_refine_ls_R_factor_gt           0.0541
_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^)+(0.0614P)^2^+3.4357P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1346
_refine_ls_wR_factor_ref         0.1417
_reflns_number_gt                10977
_reflns_number_total             12712
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            compound9.cif
_cod_data_source_block           compound9
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/current/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_cell_volume        4022.52(11)
_cod_original_sg_symbol_H-M      'P-1   '
_cod_database_code               4082651