Dearomatization reactions of N-heterocycles mediated by group 3 complexes.
Miller, Kevin L.; Williams, Bryan N.; Benitez, Diego; Carver, Colin T.; Ogilby, Kevin R.; Tkatchouk, Ekaterina; Goddard, 3rd, William A.; Diaconescu, Paula L.; Journal of the American Chemical Society 132 (2010) 342–355; doi:10.1021/ja908489p

data_4101649
_publ_section_title
;
 Dearomatization reactions of N-heterocycles mediated by group 3
 complexes.
;
_journal_issue                   1
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              342
_journal_page_last               355
_journal_paper_doi               10.1021/ja908489p
_journal_volume                  132
_journal_year                    2010
_chemical_formula_moiety         'C49 H60 Fe Lu N5 Si2, 0.5(C6 H8)'
_chemical_formula_sum            'C52 H64 Fe Lu N5 Si2'
_chemical_formula_weight         1046.08
_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                95.659(2)
_cell_angle_beta                 116.825(2)
_cell_angle_gamma                98.466(2)
_cell_formula_units_Z            2
_cell_length_a                   13.908(2)
_cell_length_b                   13.942(5)
_cell_length_c                   14.914(3)
_cell_measurement_reflns_used    7681
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.09
_cell_measurement_theta_min      3.99
_cell_volume                     2507.6(11)
_computing_cell_refinement       'Bruker APEX11'
_computing_data_collection       'Bruker APEX11'
_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      100(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.958
_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  0.0282
_diffrn_reflns_av_sigmaI/netI    0.0504
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            22108
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.35
_diffrn_reflns_theta_min         3.90
_exptl_absorpt_coefficient_mu    2.333
_exptl_absorpt_correction_T_max  0.9125
_exptl_absorpt_correction_T_min  0.7672
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs (Bruker)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.385
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1072
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.181
_refine_diff_density_min         -0.798
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     569
_refine_ls_number_reflns         12008
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.0420
_refine_ls_R_factor_gt           0.0316
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0330P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0658
_refine_ls_wR_factor_ref         0.0694
_reflns_number_gt                10156
_reflns_number_total             12008
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja908489p_si_002.cif
_cod_data_source_block           4Lu-(iqn)2
_cod_original_cell_volume        2507.6(10)
_cod_database_code               4101649