Atom-Economical Route to Substituted Pyridines via a Scandium Imide
Wicker, Benjamin F.; Scott, Jennifer; Fout, Alison R.; Pink, Maren; Mindiola, Daniel J.; Organometallics 30 (2011) 2453–; doi:10.1021/om2001537

data_4064513
_publ_section_title
;
 Atom-Economical Route to Substituted Pyridines via a Scandium Imide
;
_journal_issue                   9
_journal_name_full               Organometallics
_journal_page_first              2453
_journal_paper_doi               10.1021/om2001537
_journal_volume                  30
_journal_year                    2011
_chemical_formula_moiety         'C65 H88 N5 P2 Sc, C5 H12'
_chemical_formula_sum            'C70 H100 N5 P2 Sc'
_chemical_formula_weight         1118.45
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 94.151(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.5073(14)
_cell_length_b                   37.533(5)
_cell_length_c                   15.104(2)
_cell_measurement_reflns_used    2104
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.37
_cell_measurement_theta_min      2.41
_cell_volume                     6506.4(15)
_computing_cell_refinement       'Bruker APEX II (2009)'
_computing_data_collection       'Bruker APEX II (2009)'
_computing_data_reduction        'Bruker APEX II (2009)'
_computing_molecular_graphics    'Diamond 3.2d (2010)'
_computing_publication_material  'WinGX (2005)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 83.33
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  kappa
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1018
_diffrn_reflns_av_sigmaI/netI    0.1323
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -45
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            42263
_diffrn_reflns_theta_full        25.37
_diffrn_reflns_theta_max         25.37
_diffrn_reflns_theta_min         2.41
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'APEX II Kappa Duo'
_exptl_absorpt_coefficient_mu    0.206
_exptl_absorpt_correction_T_max  0.9918
_exptl_absorpt_correction_T_min  0.9797
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (R. Blessing, 1995)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.142
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2424
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.04
_platon_squeeze_details
;
The unit cell contains one pentane molecule which has been treated as a diffuse contribution to the overall
scattering without specific atom positions by SQUEEZE/PLATON.
;
_refine_diff_density_max         0.746
_refine_diff_density_min         -0.623
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.934
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     675
_refine_ls_number_reflns         11867
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.941
_refine_ls_R_factor_all          0.1466
_refine_ls_R_factor_gt           0.0725
_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^)+(0.0897P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1572
_refine_ls_wR_factor_ref         0.1836
_reflns_number_gt                6131
_reflns_number_total             11867
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om2001537_si_003.cif
_cod_data_source_block           4
_cod_original_cell_volume        6506.4(14)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4064513