Participation of the α,α'-Diiminopyridine Ligand System in Reduction of the Metal Center during Alkylation
Hiroyasu Sugiyama; Ghazar Aharonian; Sandro Gambarotta; Glenn P. A. Yap; Peter H. M. Budzelaar; Journal of the American Chemical Society 124 (2002) 12268–12274; doi:10.1021/ja020485m

data_4115193
_publ_section_title
;
 Participation of the \a,\a'-Diiminopyridine Ligand System in Reduction of
 the Metal Center during Alkylation
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12268
_journal_page_last               12274
_journal_paper_doi               10.1021/ja020485m
_journal_volume                  124
_journal_year                    2002
_chemical_formula_sum            'C46 H69 Al2 Cl2 Cr N3'
_chemical_formula_weight         840.90
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_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                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.9682(16)
_cell_length_b                   14.7152(13)
_cell_length_c                   19.7117(18)
_cell_measurement_reflns_used    'reflections from 60 data frames'
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      21.00
_cell_measurement_theta_min      1.47
_cell_volume                     5211.9(8)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0805
_diffrn_reflns_av_sigmaI/netI    0.1040
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            46053
_diffrn_reflns_theta_full        21.00
_diffrn_reflns_theta_max         21.00
_diffrn_reflns_theta_min         1.53
_diffrn_standards_decay_%        <1
_diffrn_standards_number         '50 standard frames at start and end'
_exptl_absorpt_coefficient_mu    0.386
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.835663
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing,R., Acta Cryst. (1995) A51 33-38.'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.072
_exptl_crystal_density_meas      0
_exptl_crystal_description       needle
_exptl_crystal_F_000             1800
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.941
_refine_diff_density_min         -0.709
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     242
_refine_ls_number_reflns         2926
_refine_ls_number_restraints     198
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.1153
_refine_ls_R_factor_gt           0.0868
_refine_ls_shift/su_max          0.015
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1370P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2663
_refine_ls_wR_factor_ref         0.3065
_reflns_number_gt                2117
_reflns_number_total             2926
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja020485m_3.cif
_cod_data_source_block           sg2046a
_cod_database_code               4115193