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_4064512
_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         'C52 H71 N4 P2 Sc, C5 H12'
_chemical_formula_sum            'C57 H83 N4 P2 Sc'
_chemical_formula_weight         931.17
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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                104.763(3)
_cell_angle_beta                 101.279(2)
_cell_angle_gamma                95.942(2)
_cell_formula_units_Z            2
_cell_length_a                   10.6222(12)
_cell_length_b                   15.5318(18)
_cell_length_c                   17.776(2)
_cell_measurement_reflns_used    2054
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.13
_cell_measurement_theta_min      1.22
_cell_volume                     2744.5(5)
_computing_cell_refinement       'Bruker APEX 2 (2009)'
_computing_data_collection       'Bruker APEX 2 (2009)'
_computing_data_reduction        'Bruker APEX 2 (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 0.987
_diffrn_measured_fraction_theta_max 0.987
_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  0.0344
_diffrn_reflns_av_sigmaI/netI    0.0413
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            49222
_diffrn_reflns_theta_full        29.13
_diffrn_reflns_theta_max         29.13
_diffrn_reflns_theta_min         1.22
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'Bruker APEX II Kappa Duo'
_exptl_absorpt_coefficient_mu    0.231
_exptl_absorpt_correction_T_max  0.9773
_exptl_absorpt_correction_T_min  0.9662
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (R. Blessing, 1995)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.127
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1008
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.961
_refine_diff_density_min         -0.498
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     604
_refine_ls_number_reflns         14601
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0753
_refine_ls_R_factor_gt           0.0514
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0725P)^2^+1.2691P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1313
_refine_ls_wR_factor_ref         0.1459
_reflns_number_gt                10749
_reflns_number_total             14601
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om2001537_si_003.cif
_cod_data_source_block           3b
_cod_original_cell_volume        2744.6(5)
_cod_database_code               4064512