Synthesis and Structural Studies of Lithium and Sodium Complexes with OOO-Tridentate Bis(phenolate) Ligands: Effective Catalysts for the Ring-Opening Polymerization of l-Lactide
Yong Huang; Yueh-Hsuan Tsai; Wen-Chou Hung; Chieh-Shen Lin; Wei Wang; Jui-Hsien Huang; Saikat Dutta; Chu-Chieh Lin; Inorganic Chemistry 49 (2010) 9416–9425; doi:10.1021/ic1011154

data_4316780
_publ_section_title
;
 Synthesis and Structural Studies of Lithium and Sodium Complexes with
 OOO-Tridentate Bis(phenolate) Ligands: Effective Catalysts for the
 Ring-Opening Polymerization of l-Lactide
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9416
_journal_page_last               9425
_journal_paper_doi               10.1021/ic1011154
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety         'C62 H68 Li2 O6,C4 O,C6'
_chemical_formula_sum            'C72 H68 Li2 O7'
_chemical_formula_weight         1059.14
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           36
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'C 2c -2'
_symmetry_space_group_name_H-M   'C m c 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                   17.0504(11)
_cell_length_b                   24.7463(17)
_cell_length_c                   15.1602(9)
_cell_measurement_reflns_used    6864
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.99
_cell_measurement_theta_min      2.389
_cell_volume                     6396.6(7)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_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      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD'
_diffrn_measurement_method       '\f and \w 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  0.0274
_diffrn_reflns_av_sigmaI/netI    0.0250
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            17255
_diffrn_reflns_theta_full        26.04
_diffrn_reflns_theta_max         26.04
_diffrn_reflns_theta_min         1.98
_exptl_absorpt_coefficient_mu    0.069
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7229
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Sheldrick (1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.100
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2248
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.510
_refine_diff_density_min         -0.182
_refine_diff_density_rms         0.052
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.6(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         6146
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0681
_refine_ls_R_factor_gt           0.0527
_refine_ls_shift/su_max          0.048
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1399
_refine_ls_wR_factor_ref         0.1519
_reflns_number_gt                4740
_reflns_number_total             6146
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic1011154_si_003.cif
_cod_data_source_block           hy08m
_cod_database_code               4316780