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_4107263
_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         '2(C39 H60 Al N4 Ni P3), C7 H8'
_chemical_formula_sum            'C85 H128 Al2 N8 Ni2 P6'
_chemical_formula_weight         1619.11
_chemical_name_common            11037
_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                70.763(6)
_cell_angle_beta                 80.530(6)
_cell_angle_gamma                82.984(6)
_cell_formula_units_Z            1
_cell_length_a                   11.228(5)
_cell_length_b                   14.192(7)
_cell_length_c                   14.309(6)
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.52
_cell_volume                     2117.8(17)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_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  0.0517
_diffrn_reflns_av_sigmaI/netI    0.0649
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            24046
_diffrn_reflns_theta_full        27.43
_diffrn_reflns_theta_max         27.43
_diffrn_reflns_theta_min         1.52
_exptl_absorpt_coefficient_mu    0.627
_exptl_absorpt_correction_T_max  0.9400
_exptl_absorpt_correction_T_min  0.8849
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, R. Blessing, 1995'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.270
_exptl_crystal_description       plate
_exptl_crystal_F_000             866
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.561
_refine_diff_density_min         -0.369
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.940
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     474
_refine_ls_number_reflns         9491
_refine_ls_number_restraints     34
_refine_ls_restrained_S_all      0.941
_refine_ls_R_factor_all          0.0561
_refine_ls_R_factor_gt           0.0363
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0384P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0813
_refine_ls_wR_factor_ref         0.0877
_reflns_number_gt                6939
_reflns_number_total             9491
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja2099744_si_003.cif
_cod_data_source_block           Compound3
_cod_original_cell_volume        2117.7(17)
_cod_database_code               4107263