The synthesis of a dichloroalane complex and its reaction with an α-diimine
Alexander, Sean G.; Cole, Marcus L.; Hilder, Matthias; Morris, Jonathan C.; Patrick, Joanna B.; Dalton Transactions  (2008) 6361–6363; doi:10.1039/B814839b

data_7004810
_publ_section_title
;
 The synthesis of a dichloroalane complex and its reaction with an
 \a-diimine
;
_journal_issue                   45
_journal_name_full               'Dalton Transactions'
_journal_page_first              6361
_journal_page_last               6363
_journal_paper_doi               10.1039/B814839b
_journal_year                    2008
_chemical_compound_source        THF-Hexane
_chemical_formula_moiety         'C41 H47 Al Cl2 N4'
_chemical_formula_sum            'C41 H47 Al Cl2 N4'
_chemical_formula_weight         693.71
_chemical_melting_point          603
_chemical_name_common            (AlCl2(MesNC(=IMes)C(H)NMes))
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 91.942(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.0810(2)
_cell_length_b                   18.3266(4)
_cell_length_c                   21.1938(4)
_cell_measurement_reflns_used    47016
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      28.35
_cell_measurement_theta_min      3.53
_cell_volume                     3913.32(14)
_computing_cell_refinement       DENZO-SMN
_computing_data_collection       'Nonius Collect'
_computing_data_reduction        X-Seed
_computing_molecular_graphics    'X-Seed / POV-Ray'
_computing_publication_material  'Microsoft Office 2000'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       'psi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1163
_diffrn_reflns_av_sigmaI/netI    0.1473
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            47016
_diffrn_reflns_theta_full        28.35
_diffrn_reflns_theta_max         28.35
_diffrn_reflns_theta_min         3.53
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.221
_exptl_absorpt_correction_T_max  0.9167
_exptl_absorpt_correction_T_min  0.8429
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow-orange
_exptl_crystal_density_diffrn    1.177
_exptl_crystal_density_method    none
_exptl_crystal_description       prism
_exptl_crystal_F_000             1472
_exptl_crystal_size_max          0.80
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.424
_refine_diff_density_min         -0.438
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     445
_refine_ls_number_reflns         9591
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.1932
_refine_ls_R_factor_gt           0.0961
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1439P)^2^+0.3514P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2069
_refine_ls_wR_factor_ref         0.2571
_reflns_number_gt                5219
_reflns_number_total             9591
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            B814839b.txt
_cod_data_source_block           COMPOUND_4
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7004810