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_7024324
_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_sum            'C16 H25 N5 S'
_chemical_formula_weight         319.47
_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                89.887(3)
_cell_angle_beta                 83.512(3)
_cell_angle_gamma                75.696(2)
_cell_formula_units_Z            2
_cell_length_a                   8.6457(13)
_cell_length_b                   9.4203(14)
_cell_length_c                   11.1657(17)
_cell_measurement_temperature    180(2)
_cell_volume                     875.2(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX'
_computing_data_reduction        'Bruker SHELXTL'
_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 0.732
_diffrn_measured_fraction_theta_max 0.732
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'omega scan'
_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  0.0558
_diffrn_reflns_av_sigmaI/netI    0.0626
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            4266
_diffrn_reflns_theta_full        26.46
_diffrn_reflns_theta_max         26.46
_diffrn_reflns_theta_min         1.84
_exptl_absorpt_coefficient_mu    0.190
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.581279
_exptl_absorpt_correction_type   Semi-empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.212
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Needle
_exptl_crystal_F_000             344
_exptl_crystal_size_max          0.428
_exptl_crystal_size_mid          0.411
_exptl_crystal_size_min          0.154
_refine_diff_density_max         0.289
_refine_diff_density_min         -0.319
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.143
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     210
_refine_ls_number_reflns         2645
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.143
_refine_ls_R_factor_all          0.0763
_refine_ls_R_factor_gt           0.0530
_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^)+(0.0818P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1424
_refine_ls_wR_factor_ref         0.1591
_reflns_number_gt                1912
_reflns_number_total             2645
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b914966j.txt
_cod_data_source_block           6
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7024324