Design of new heteroscorpionate ligands and their coordinative ability toward Group 4 transition metals; an efficient synthetic route to obtain enantiopure ligands.
Otero, Antonio; Fernández-Baeza, Juan; Antiñolo, Antonio; Tejeda, Juan; Lara-Sánchez, Agustín; Sánchez-Barba, Luis; Sánchez-Molina, Margarita; Franco, Sonia; López-Solera, Isabel; Rodríguez, Ana M; Dalton transactions (Cambridge, England : 2003)  (2006) 4359–4370; doi:10.1039/b605703a

data_7007461
_publ_section_title
;
 Design of new heteroscorpionate ligands and their coordinative ability
 toward Group 4 transition metals; an efficient synthetic route to
 obtain enantiopure ligands.
;
_journal_issue                   36
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4359
_journal_page_last               4370
_journal_paper_doi               10.1039/b605703a
_journal_year                    2006
_chemical_formula_sum            'C19 H32 Li N5 O S Si'
_chemical_formula_weight         413.59
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.185(2)
_cell_length_b                   8.806(3)
_cell_length_c                   14.696(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    290(2)
_cell_measurement_theta_max      20
_cell_measurement_theta_min      2
_cell_volume                     2482.8(9)
_computing_cell_refinement       'Nonius (control program)'
_computing_data_collection       'Nonius (control program)'
_computing_data_reduction        'XRAY80 (Stewart, 1976)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      290(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'four circle diffractometer Nonius-Mach3'
_diffrn_measurement_method       '\w/2\q 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  0.0441
_diffrn_reflns_av_sigmaI/netI    0.1449
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            6226
_diffrn_reflns_theta_full        27.99
_diffrn_reflns_theta_max         27.99
_diffrn_reflns_theta_min         2.12
_diffrn_standards_interval_time  60
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.195
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.106
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             888
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.208
_refine_diff_density_min         -0.220
_refine_diff_density_rms         0.047
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.13(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     257
_refine_ls_number_reflns         5992
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.2360
_refine_ls_R_factor_gt           0.0769
_refine_ls_shift/su_max          0.044
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1046P)^2^+0.2502P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1852
_refine_ls_wR_factor_ref         0.2391
_reflns_number_gt                2460
_reflns_number_total             5992
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b605703a.txt
_cod_data_source_block           12
_cod_original_sg_symbol_H-M      Pna21
_cod_database_code               7007461