Synthetic, Structural, Mechanistic, and Computational Studies on Single-Site β-Diketiminate Tin(II) Initiators for the Polymerization of rac-Lactide
Andrew P. Dove; Vernon C. Gibson; Edward L. Marshall; Henry S. Rzepa; Andrew J. P. White; David J. Williams; Journal of the American Chemical Society 128 (2006) 9834–9843; doi:10.1021/ja061400a

data_4110753
_publ_section_title
;
 Synthetic, Structural, Mechanistic, and Computational Studies on
 Single-Site \b-Diketiminate Tin(II) Initiators for the Polymerization of
 rac-Lactide
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9834
_journal_page_last               9843
_journal_paper_doi               10.1021/ja061400a
_journal_volume                  128
_journal_year                    2006
_chemical_formula_sum            'C35 H52 N2 O3 Sn'
_chemical_formula_weight         667.48
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 109.008(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.7495(19)
_cell_length_b                   9.8141(18)
_cell_length_c                   16.5355(19)
_cell_measurement_reflns_used    23
_cell_measurement_temperature    203(2)
_cell_measurement_theta_max      11.52
_cell_measurement_theta_min      5.31
_cell_volume                     1802.8(5)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_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      203(2)
_diffrn_measured_fraction_theta_full 0.929
_diffrn_measured_fraction_theta_max 0.929
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\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  0.0318
_diffrn_reflns_av_sigmaI/netI    0.0591
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            3303
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.45
_diffrn_standards_decay_%        10.23
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.741
_exptl_absorpt_correction_T_max  0.9601
_exptl_absorpt_correction_T_min  0.7971
_exptl_absorpt_correction_type   'Lamina [1 0 -1]'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.230
_exptl_crystal_description       'platy needles'
_exptl_crystal_F_000             700
_exptl_crystal_size_max          0.93
_exptl_crystal_size_mid          0.37
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.497
_refine_diff_density_min         -0.366
_refine_diff_density_rms         0.068
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.02(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     372
_refine_ls_number_reflns         3133
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.0455
_refine_ls_R_factor_gt           0.0347
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0327P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0728
_refine_ls_wR_factor_ref         0.0762
_reflns_number_gt                2731
_reflns_number_total             3133
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja061400asi20060308_075058_4.cif
_cod_data_source_block           Compound_14
_cod_database_code               4110753