σ-Alane Complexes of Chromium, Tungsten, and Manganese
Ian M. Riddlestone; Siân Edmonds; Paul A. Kaufman; Juan Urbano Baena; Joshua I. Bates; Michael J. Kelly; Amber L. Thompson; Russell Taylor; Simon Aldridge; Journal of the American Chemical Society 134 (2012) 2551–2554; doi:10.1021/ja2119892

data_4117441
_publ_contact_author             'Simon Aldridge'
_publ_contact_author_email       Simon.aldridge@chem.ox.ac.uk
_publ_section_title
;
 \s-Alane Complexes of Chromium, Tungsten, and Manganese
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2551
_journal_page_last               2554
_journal_paper_doi               10.1021/ja2119892
_journal_volume                  134
_journal_year                    2012
_chemical_formula_moiety         'C20 H24 Al1 Cl1 Fe1 N2 O2'
_chemical_formula_sum            'C20 H24 Al Cl Fe N2 O2'
_chemical_formula_weight         442.70
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             10-06-02
_audit_creation_method           CRYSTALS_ver_14.03
_cell_angle_alpha                90
_cell_angle_beta                 93.0773(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.9088(2)
_cell_length_b                   12.3092(3)
_cell_length_c                   17.7168(4)
_cell_measurement_reflns_used    4943
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     2157.79(8)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.033
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            9335
_diffrn_reflns_theta_full        26.388
_diffrn_reflns_theta_max         27.487
_diffrn_reflns_theta_min         5.101
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.880
_exptl_absorpt_correction_T_max  0.92
_exptl_absorpt_correction_T_min  0.92
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.363
_exptl_crystal_description       block
_exptl_crystal_F_000             920
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.90
_refine_diff_density_min         -0.78
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.9274
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         4907
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0675
_refine_ls_R_factor_gt           0.0458
_refine_ls_shift/su_max          0.0010660
_refine_ls_shift/su_mean         4.7106056
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.10P)^2^ + 0.00P] 
 ,where P=p(6)*max(Fo^2^,0) + (1-p(6))Fc^2^ 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1365
_refine_ls_wR_factor_gt          0.1224
_refine_ls_wR_factor_ref         0.1365
_reflns_limit_h_max              12
_reflns_limit_h_min              -12
_reflns_limit_k_max              15
_reflns_limit_k_min              0
_reflns_limit_l_max              22
_reflns_limit_l_min              0
_reflns_number_gt                3672
_reflns_number_total             4907
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.34
_oxford_diffrn_Wilson_scale      16.53
_oxford_refine_ls_r_factor_ref   0.0675
_oxford_refine_ls_scale          0.2371(3)
_oxford_reflns_number_all        4907
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title 051irdv10
_cod_data_source_file            ja2119892_si_002_1.cif
_cod_data_source_block           Fe
_cod_original_sg_symbol_H-M      'P 1 21/c 1 '
_cod_original_formula_sum        'C20 H24 Al1 Cl1 Fe1 N2 O2'
_cod_database_code               4117441