#------------------------------------------------------------------------------
#$Date: 2016-03-22 10:37:57 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178878 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/07/4110751.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4110751
loop_
_publ_author_name
'Andrew P. Dove'
'Vernon C. Gibson'
'Edward L. Marshall'
'Henry S. Rzepa'
'Andrew J. P. White'
'David J. Williams'
_publ_section_title
;
 Synthetic, Structural, Mechanistic, and Computational Studies on
 Single-Site β-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            'C20 H24 N2 O Sn'
_chemical_formula_weight         427.10
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 96.196(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.2919(13)
_cell_length_b                   10.6268(9)
_cell_length_c                   25.237(3)
_cell_measurement_reflns_used    30
_cell_measurement_temperature    203(2)
_cell_measurement_theta_max      22.53
_cell_measurement_theta_min      11.06
_cell_volume                     1944.2(4)
_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 0.843
_diffrn_measured_fraction_theta_max 0.843
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω 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  0.0332
_diffrn_reflns_av_sigmaI/netI    0.0370
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            2660
_diffrn_reflns_theta_full        59.50
_diffrn_reflns_theta_max         59.50
_diffrn_reflns_theta_min         3.52
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    10.506
_exptl_absorpt_correction_T_max  0.6158
_exptl_absorpt_correction_T_min  0.1438
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.459
_exptl_crystal_description       'platy needles'
_exptl_crystal_F_000             864
_exptl_crystal_size_max          0.73
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.847
_refine_diff_density_min         -1.052
_refine_diff_density_rms         0.180
_refine_ls_extinction_coef       0.00013(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.158
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     196
_refine_ls_number_reflns         2396
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.158
_refine_ls_R_factor_all          0.0811
_refine_ls_R_factor_gt           0.0574
_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/[σ²(Fo²)+(0.0338P)²+35.9937P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1416
_refine_ls_wR_factor_ref         0.1585
_reflns_number_gt                1978
_reflns_number_total             2396
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja061400asi20060308_075058_2.cif
_cod_data_source_block           Compound_9
_cod_database_code               4110751
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Sn Sn 0.86324(11) 0.45200(7) 0.18582(3) 0.0284(3) Uani 1 1 d .
C1 C 1.2674(17) 0.5634(11) 0.2153(4) 0.032(3) Uani 1 1 d .
N1 N 1.1074(14) 0.5321(10) 0.2315(4) 0.035(2) Uani 1 1 d .
C2 C 1.3168(16) 0.5429(12) 0.1637(4) 0.033(3) Uani 1 1 d .
H2A H 1.4215 0.5859 0.1545 0.039 Uiso 1 1 calc R
C3 C 1.2262(18) 0.4652(12) 0.1245(4) 0.035(3) Uani 1 1 d .
N3 N 1.0572(13) 0.4179(9) 0.1267(3) 0.028(2) Uani 1 1 d .
C4 C 1.410(2) 0.6336(14) 0.2532(5) 0.048(3) Uani 1 1 d .
H4A H 1.3490 0.6724 0.2814 0.073 Uiso 1 1 calc R
H4B H 1.4684 0.6981 0.2337 0.073 Uiso 1 1 calc R
H4C H 1.5024 0.5748 0.2686 0.073 Uiso 1 1 calc R
C5 C 1.3254(19) 0.4394(15) 0.0761(5) 0.048(3) Uani 1 1 d .
H5A H 1.3756 0.3547 0.0782 0.072 Uiso 1 1 calc R
H5B H 1.4250 0.4995 0.0747 0.072 Uiso 1 1 calc R
H5C H 1.2394 0.4473 0.0441 0.072 Uiso 1 1 calc R
C6 C 1.0869(11) 0.5355(7) 0.2879(2) 0.031(3) Uani 1 1 d G
C7 C 0.9718(12) 0.6242(7) 0.3077(3) 0.043(3) Uani 1 1 d G
H7A H 0.9150 0.6862 0.2849 0.052 Uiso 1 1 calc R
C8 C 0.9406(12) 0.6212(7) 0.3610(3) 0.048(4) Uani 1 1 d G
H8A H 0.8628 0.6813 0.3744 0.057 Uiso 1 1 calc R
C9 C 1.0246(12) 0.5295(8) 0.3946(2) 0.047(3) Uani 1 1 d G
H9A H 1.0035 0.5275 0.4307 0.057 Uiso 1 1 calc R
C10 C 1.1397(12) 0.4408(7) 0.3749(2) 0.043(3) Uani 1 1 d G
H10A H 1.1964 0.3788 0.3976 0.051 Uiso 1 1 calc R
C11 C 1.1708(10) 0.4438(6) 0.3215(3) 0.035(3) Uani 1 1 d G
H11A H 1.2486 0.3837 0.3082 0.042 Uiso 1 1 calc R
C12 C 0.9840(11) 0.3261(6) 0.0884(3) 0.038(3) Uani 1 1 d G
C13 C 1.0477(10) 0.2028(7) 0.0903(3) 0.039(3) Uani 1 1 d G
H13A H 1.1479 0.1798 0.1150 0.047 Uiso 1 1 calc R
C14 C 0.9631(12) 0.1133(5) 0.0556(3) 0.043(3) Uani 1 1 d G
H14A H 1.0062 0.0298 0.0569 0.052 Uiso 1 1 calc R
C15 C 0.8149(12) 0.1472(7) 0.0191(3) 0.047(4) Uani 1 1 d G
H15A H 0.7577 0.0867 -0.0043 0.057 Uiso 1 1 calc R
C16 C 0.7512(11) 0.2706(8) 0.0173(3) 0.049(4) Uani 1 1 d G
H16A H 0.6509 0.2935 -0.0074 0.059 Uiso 1 1 calc R
C17 C 0.8357(12) 0.3600(6) 0.0519(3) 0.046(3) Uani 1 1 d G
H17A H 0.7927 0.4435 0.0507 0.055 Uiso 1 1 calc R
O20 O 0.7644(12) 0.6091(8) 0.1508(3) 0.041(2) Uani 1 1 d .
C21 C 0.859(2) 0.7113(12) 0.1301(5) 0.047(3) Uani 1 1 d .
H21A H 0.9894 0.6863 0.1288 0.056 Uiso 1 1 calc R
C22 C 0.856(2) 0.8255(12) 0.1646(5) 0.051(4) Uani 1 1 d .
H22A H 0.9098 0.8055 0.2004 0.077 Uiso 1 1 calc R
H22B H 0.7290 0.8526 0.1656 0.077 Uiso 1 1 calc R
H22C H 0.9255 0.8925 0.1501 0.077 Uiso 1 1 calc R
C23 C 0.777(3) 0.7411(13) 0.0744(5) 0.072(6) Uani 1 1 d .
H23A H 0.7814 0.6668 0.0522 0.107 Uiso 1 1 calc R
H23B H 0.8460 0.8086 0.0601 0.107 Uiso 1 1 calc R
H23C H 0.6494 0.7670 0.0750 0.107 Uiso 1 1 calc R
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sn Sn 0.0259 5.4591 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
O20 Sn N1 98.2(4)
O20 Sn N3 93.8(3)
N1 Sn N3 82.8(3)
N1 C1 C2 124.9(11)
N1 C1 C4 119.5(10)
C2 C1 C4 115.6(11)
C1 N1 C6 119.2(9)
C1 N1 Sn 129.1(7)
C6 N1 Sn 111.3(6)
C3 C2 C1 126.8(12)
N3 C3 C2 124.1(11)
N3 C3 C5 119.2(11)
C2 C3 C5 116.7(12)
C3 N3 C12 120.4(9)
C3 N3 Sn 129.1(8)
C12 N3 Sn 110.5(6)
C7 C6 C11 120.0
C7 C6 N1 120.0(6)
C11 C6 N1 119.8(6)
C8 C7 C6 120.0
C7 C8 C9 120.0
C10 C9 C8 120.0
C9 C10 C11 120.0
C10 C11 C6 120.0
C13 C12 C17 120.0
C13 C12 N3 121.3(6)
C17 C12 N3 118.5(6)
C12 C13 C14 120.0
C13 C14 C15 120.0
C16 C15 C14 120.0
C15 C16 C17 120.0
C16 C17 C12 120.0
C21 O20 Sn 129.8(8)
O20 C21 C22 111.6(11)
O20 C21 C23 110.1(13)
C22 C21 C23 110.1(11)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Sn O20 1.987(8)
Sn N1 2.187(10)
Sn N3 2.194(9)
C1 N1 1.320(16)
C1 C2 1.405(16)
C1 C4 1.528(17)
N1 C6 1.448(10)
C2 C3 1.397(17)
C3 N3 1.338(16)
C3 C5 1.512(16)
N3 C12 1.435(10)
C6 C7 1.3900
C6 C11 1.3900
C7 C8 1.3900
C8 C9 1.3900
C9 C10 1.3900
C10 C11 1.3900
C12 C13 1.3900
C12 C17 1.3900
C13 C14 1.3900
C14 C15 1.3900
C15 C16 1.3900
C16 C17 1.3900
O20 C21 1.417(15)
C21 C22 1.495(19)
C21 C23 1.502(19)
