Metal-Alane Adducts with Zero-Valent Nickel, Cobalt, and Iron
P. Alex Rudd; Shengsi Liu; Laura Gagliardi; Victor G. Young; Connie C. Lu; Journal of the American Chemical Society 133 (2011) 20724–20727; doi:10.1021/ja2099744

data_4107265
_publ_section_title
;
 Metal-Alane Adducts with Zero-Valent Nickel, Cobalt, and Iron
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              20724
_journal_page_last               20727
_journal_paper_doi               10.1021/ja2099744
_journal_volume                  133
_journal_year                    2011
_chemical_formula_moiety         'C78 H120 Al2 Fe2 N10 P6'
_chemical_formula_sum            'C78 H120 Al2 Fe2 N10 P6'
_chemical_formula_weight         1549.32
_chemical_name_common            11201
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           182
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  'P 6c 2c'
_symmetry_space_group_name_H-M   'P 63 2 2'
_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                120.00
_cell_formula_units_Z            2
_cell_length_a                   15.5732(19)
_cell_length_b                   15.5732(19)
_cell_length_c                   25.258(3)
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      24.98
_cell_volume                     5305.0(11)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0254
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3123
_diffrn_reflns_theta_full        24.98
_diffrn_reflns_theta_max         24.98
_diffrn_reflns_theta_min         1.71
_exptl_absorpt_coefficient_mu    0.417
_exptl_absorpt_correction_T_max  0.9595
_exptl_absorpt_correction_T_min  0.9212
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, R. Blessing, 1995'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    0.970
_exptl_crystal_description       needle
_exptl_crystal_F_000             1652
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.262
_refine_diff_density_min         -0.303
_refine_diff_density_rms         0.058
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.01(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     152
_refine_ls_number_reflns         3123
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0620
_refine_ls_R_factor_gt           0.0470
_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^)+(0.0948P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1333
_refine_ls_wR_factor_ref         0.1420
_reflns_number_gt                2348
_reflns_number_total             3123
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja2099744_si_005.cif
_cod_data_source_block           11201zz
_cod_database_code               4107265