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_4110750
_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            'C31 H47 N3 Sn'
_chemical_formula_weight         580.41
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 99.725(15)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.9672(13)
_cell_length_b                   22.516(2)
_cell_length_c                   15.026(2)
_cell_measurement_reflns_used    33
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      11.08
_cell_volume                     2990.2(7)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      183(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0312
_diffrn_reflns_av_sigmaI/netI    0.0371
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            2742
_diffrn_reflns_theta_max         64.01
_diffrn_reflns_theta_min         2.98
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    6.947
_exptl_absorpt_correction_T_max  0.2109
_exptl_absorpt_correction_T_min  0.1031
_exptl_absorpt_correction_type   Ellipsoidal
_exptl_crystal_colour            Yellow/orange
_exptl_crystal_density_diffrn    1.289
_exptl_crystal_description       blocks
_exptl_crystal_F_000             1216
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.469
_refine_diff_density_min         -0.820
_refine_diff_density_rms         0.068
_refine_ls_extinction_coef       0.00028(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.073
_refine_ls_goodness_of_fit_obs   1.089
_refine_ls_matrix_type           full
_refine_ls_number_parameters     175
_refine_ls_number_reflns         2512
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.139
_refine_ls_restrained_S_obs      1.146
_refine_ls_R_factor_all          0.0369
_refine_ls_R_factor_obs          0.0327
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0490P)^2^+1.2620P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0841
_refine_ls_wR_factor_obs         0.0810
_reflns_number_observed          2368
_reflns_number_total             2562
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja061400asi20060308_075058_1.cif
_cod_data_source_block           Compound_3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0490P)^2^+1.2620P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0490P)^2^+1.2620P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        2990.3(6)
_cod_database_code               4110750