#------------------------------------------------------------------------------
#$Date: 2016-03-22 10:37:57 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178878 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/07/4110750.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_4110750
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            '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       '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  0.0312
_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+0.001xFc²λ³/sin(2θ)]^-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/[σ²(Fo²)+(0.0490P)²+1.2620P] where P=(Fo²+2Fc²)/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
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Sn Sn 0.66425(3) 0.0000 0.21556(2) 0.03653(14) Uani 1 d S .
C1 C 0.4316(4) -0.0561(2) 0.3323(2) 0.0404(7) Uani 1 d . .
N1 N 0.5135(3) -0.06540(13) 0.2671(2) 0.0372(6) Uani 1 d . .
C2 C 0.4046(5) 0.0000 0.3655(3) 0.0431(11) Uani 1 d S .
H2A H 0.3613(5) 0.0000 0.4190(3) 0.052 Uiso 1 calc SR .
C3 C 0.3618(5) -0.1082(2) 0.3726(3) 0.0555(9) Uani 1 d . .
H3A H 0.3136(5) -0.0945(2) 0.4228(3) 0.083 Uiso 1 d R .
H3B H 0.4406(5) -0.1373(2) 0.3949(3) 0.083 Uiso 1 d R .
H3C H 0.2858(5) -0.1267(2) 0.3264(3) 0.083 Uiso 1 d R .
C4 C 0.5150(4) -0.1227(2) 0.2251(2) 0.0424(7) Uani 1 d . .
C5 C 0.4092(5) -0.1344(2) 0.1465(3) 0.0562(10) Uani 1 d . .
C6 C 0.4165(7) -0.1895(2) 0.1050(3) 0.078(2) Uani 1 d . .
H6A H 0.3457(7) -0.1981(2) 0.0521(3) 0.093 Uiso 1 calc R .
C7 C 0.5207(8) -0.2311(2) 0.1372(4) 0.083(2) Uani 1 d . .
H7A H 0.5210(8) -0.2685(2) 0.1078(4) 0.100 Uiso 1 calc R .
C8 C 0.6251(7) -0.2191(2) 0.2121(4) 0.0697(12) Uani 1 d . .
H8A H 0.6998(7) -0.2480(2) 0.2334(4) 0.084 Uiso 1 calc R .
C9 C 0.6248(5) -0.1651(2) 0.2583(3) 0.0502(8) Uani 1 d . .
C10 C 0.2966(6) -0.0889(2) 0.1054(3) 0.0745(15) Uani 1 d D .
H10A H 0.3478(6) -0.0493(2) 0.1128(3) 0.089 Uiso 0.55 calc PR 1
H10B H 0.3236(6) -0.0537(2) 0.1454(3) 0.089 Uiso 0.45 d PR 2
C11 C 0.1652(11) -0.0847(5) 0.1430(6) 0.067(2) Uani 0.55 d PD 1
H11A H 0.0995(11) -0.0538(5) 0.1115(6) 0.101 Uiso 0.55 calc PR 1
H11B H 0.1916(11) -0.0745(5) 0.2071(6) 0.101 Uiso 0.55 calc PR 1
H11C H 0.1120(11) -0.1229(5) 0.1368(6) 0.101 Uiso 0.55 calc PR 1
C12 C 0.2585(11) -0.1033(5) -0.0031(5) 0.070(2) Uani 0.55 d PD 1
H12A H 0.3532(11) -0.1059(5) -0.0273(5) 0.105 Uiso 0.55 calc PR 1
H12B H 0.1957(11) -0.0714(5) -0.0340(5) 0.105 Uiso 0.55 calc PR 1
H12C H 0.2040(11) -0.1411(5) -0.0128(5) 0.105 Uiso 0.55 calc PR 1
C11' C 0.1234(14) -0.1056(6) 0.1218(9) 0.067(3) Uiso 0.45 d PD 2
H11D H 0.1281(14) -0.1232(6) 0.1819(9) 0.101 Uiso 0.45 calc PR 2
H11E H 0.0778(14) -0.1340(6) 0.0758(9) 0.101 Uiso 0.45 calc PR 2
H11F H 0.0619(14) -0.0694(6) 0.1175(9) 0.101 Uiso 0.45 calc PR 2
C12' C 0.2875(13) -0.0640(5) 0.0198(7) 0.062(2) Uiso 0.45 d PD 2
H12D H 0.2039(13) -0.0354(5) 0.0095(7) 0.093 Uiso 0.45 calc PR 2
H12E H 0.2696(13) -0.0954(5) -0.0259(7) 0.093 Uiso 0.45 calc PR 2
H12F H 0.3826(13) -0.0436(5) 0.0155(7) 0.093 Uiso 0.45 calc PR 2
C13 C 0.7428(5) -0.1549(2) 0.3407(3) 0.0605(10) Uani 1 d . .
H13A H 0.7242(5) -0.1148(2) 0.3654(3) 0.073 Uiso 1 calc R .
C14 C 0.9018(6) -0.1547(3) 0.3173(5) 0.091(2) Uani 1 d . .
H14A H 0.9760(6) -0.1479(3) 0.3722(5) 0.137 Uiso 1 calc R .
H14B H 0.9099(6) -0.1230(3) 0.2737(5) 0.137 Uiso 1 calc R .
H14C H 0.9218(6) -0.1931(3) 0.2909(5) 0.137 Uiso 1 calc R .
C15 C 0.7333(8) -0.2009(3) 0.4153(4) 0.083(2) Uani 1 d . .
H15A H 0.8119(8) -0.1925(3) 0.4675(4) 0.124 Uiso 1 calc R .
H15B H 0.7484(8) -0.2408(3) 0.3924(4) 0.124 Uiso 1 calc R .
H15C H 0.6336(8) -0.1986(3) 0.4335(4) 0.124 Uiso 1 calc R .
N16 N 0.8273(5) 0.0000 0.3299(3) 0.0480(10) Uani 1 d S .
C17 C 0.9847(6) 0.0000 0.3217(5) 0.062(2) Uani 1 d S .
H17A H 1.0354(6) -0.0338 0.3551(5) 0.093 Uiso 0.50 d PR .
H17B H 1.0318(6) 0.0371 0.3466(5) 0.093 Uiso 0.50 d PR .
H17C H 0.9943(6) 0.0000 0.2579(5) 0.093 Uiso 1 d SR .
C18 C 0.8065(6) 0.0000 0.4220(4) 0.0579(15) Uani 1 d S .
H18A H 0.8640(6) 0.0328 0.4541(4) 0.087 Uiso 0.50 d PR .
H18B H 0.8425(6) -0.0377 0.4503(4) 0.087 Uiso 0.50 d PR .
H18C H 0.6988(6) 0.0049 0.4248(4) 0.087 Uiso 0.50 d PR .
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'
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
_geom_angle_site_symmetry_3
N16 Sn N1 95.59(12) .
N16 Sn N1 95.59(12) 6
N1 Sn N1 82.91(15) 6
N1 C1 C2 123.7(3) .
N1 C1 C3 119.4(3) .
C2 C1 C3 116.9(3) .
C1 N1 C4 120.6(3) .
C1 N1 Sn 126.4(2) .
C4 N1 Sn 113.0(2) .
C1 C2 C1 129.8(4) 6
C9 C4 C5 120.2(4) .
C9 C4 N1 120.9(3) .
C5 C4 N1 118.8(4) .
C6 C5 C4 117.8(5) .
C6 C5 C10 120.3(4) .
C4 C5 C10 121.9(4) .
C7 C6 C5 122.5(5) .
C6 C7 C8 119.5(5) .
C7 C8 C9 121.5(5) .
C8 C9 C4 118.4(4) .
C8 C9 C13 118.8(4) .
C4 C9 C13 122.8(4) .
C11 C10 C5 115.9(6) .
C12' C10 C5 125.9(7) .
C11 C10 C12 111.6(6) .
C5 C10 C12 106.7(6) .
C12' C10 C11' 108.6(7) .
C5 C10 C11' 111.6(6) .
C9 C13 C14 111.4(4) .
C9 C13 C15 112.2(4) .
C14 C13 C15 109.8(4) .
C18 N16 C17 111.9(5) .
C18 N16 Sn 128.2(3) .
C17 N16 Sn 119.9(4) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Sn N16 2.059(4) .
Sn N1 2.224(3) .
Sn N1 2.224(3) 6
C1 N1 1.337(4) .
C1 C2 1.394(4) .
C1 C3 1.504(5) .
N1 C4 1.437(5) .
C2 C1 1.394(4) 6
C4 C9 1.401(6) .
C4 C5 1.409(5) .
C5 C6 1.394(7) .
C5 C10 1.497(7) .
C6 C7 1.353(9) .
C7 C8 1.364(8) .
C8 C9 1.400(6) .
C9 C13 1.505(6) .
C10 C11 1.393(10) .
C10 C12' 1.394(10) .
C10 C12 1.641(9) .
C10 C11' 1.656(12) .
C13 C14 1.525(7) .
C13 C15 1.539(7) .
N16 C18 1.428(7) .
N16 C17 1.438(7) .
