New achiral and chiral NNE heteroscorpionate ligands. Synthesis of homoleptic lithium complexes as well as halide and alkyl scandium and yttrium complexes.
Otero, Antonio; Lara-Sánchez, Agustín; Fernández-Baeza, Juan; Martínez-Caballero, Emilia; Márquez-Segovia, Isabel; Alonso-Moreno, Carlos; Sánchez-Barba, Luis F; Rodríguez, Ana M; López-Solera, Isabel; Dalton transactions (Cambridge, England : 2003) 39 (2010) 930–940; doi:10.1039/b914966j

data_7024323
_publ_section_title
;
 New achiral and chiral NNE heteroscorpionate ligands. Synthesis of
 homoleptic lithium complexes as well as halide and alkyl scandium and
 yttrium complexes.
;
_journal_issue                   3
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              930
_journal_page_last               940
_journal_paper_doi               10.1039/b914966j
_journal_volume                  39
_journal_year                    2010
_chemical_formula_moiety         'C18 H21 N5 S'
_chemical_formula_sum            'C18 H21 N5 S'
_chemical_formula_weight         339.46
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 90.43(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.048(2)
_cell_length_b                   11.477(2)
_cell_length_c                   13.263(5)
_cell_measurement_reflns_used    437
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      16.74
_cell_measurement_theta_min      2.33
_cell_volume                     1833.9(8)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX'
_computing_data_reduction        'Bruker SAINT, SADABS, XPREP'
_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      180(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       '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  0.1204
_diffrn_reflns_av_sigmaI/netI    0.2540
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            9267
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.28
_exptl_absorpt_coefficient_mu    0.185
_exptl_absorpt_correction_T_max  0.951
_exptl_absorpt_correction_T_min  0.923
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.229
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             720
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.181
_refine_diff_density_min         -0.209
_refine_diff_density_rms         0.041
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.844
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     225
_refine_ls_number_reflns         3192
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.844
_refine_ls_R_factor_all          0.1916
_refine_ls_R_factor_gt           0.0561
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0993P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1301
_refine_ls_wR_factor_ref         0.1905
_reflns_number_gt                836
_reflns_number_total             3192
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b914966j.txt
_cod_data_source_block           5
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               7024323