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#$Date: 2016-03-25 14:58:04 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179908 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/04/7020485.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_7020485
loop_
_publ_author_name
'Piromjitpong, Parichat'
'Ratanapanee, Passachon'
'Thumrongpatanaraks, Wipavee'
'Kongsaeree, Palangpon'
'Phomphrai, Khamphee'
_publ_section_title
;
 Synthesis of cyclic polylactide catalysed by
 bis(salicylaldiminato)tin(ii) complexes.
;
_journal_issue                   41
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12704
_journal_page_last               12710
_journal_paper_doi               10.1039/c2dt31678a
_journal_volume                  41
_journal_year                    2012
_chemical_absolute_configuration unk
_chemical_compound_source        Synthesis
_chemical_formula_moiety         'C38 H44 N2 O2 Sn'
_chemical_formula_sum            'C38 H44 N2 O2 Sn'
_chemical_formula_weight         679.472
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.977(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.8207(4)
_cell_length_b                   17.2625(5)
_cell_length_c                   23.1793(10)
_cell_measurement_reflns_used    3353
_cell_measurement_temperature    150
_cell_measurement_theta_max      28.700
_cell_measurement_theta_min      0.998
_cell_volume                     3528.9(2)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       KappaCCD
_computing_data_reduction
'Denzo and Scalepak (Otwinowski & Minor, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution
'SIR97(Cascarano al.,Acta Cryst.,1996,A52,C-79)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.960
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_device       KappaCCD
_diffrn_measurement_method       CCD
_diffrn_orient_matrix_type       X=UH
_diffrn_orient_matrix_UB_11      0.02415
_diffrn_orient_matrix_UB_12      0.11054
_diffrn_orient_matrix_UB_13      0.00732
_diffrn_orient_matrix_UB_21      0.00195
_diffrn_orient_matrix_UB_22      0.00340
_diffrn_orient_matrix_UB_23      -0.05780
_diffrn_orient_matrix_UB_31      -0.04197
_diffrn_orient_matrix_UB_32      0.00998
_diffrn_orient_matrix_UB_33      -0.00083
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           ' MoK\a'
_diffrn_radiation_wavelength_id  all
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            7069
_diffrn_reflns_theta_full        28.71
_diffrn_reflns_theta_max         28.71
_diffrn_reflns_theta_min         1.76
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.757
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.279
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1408
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.600
_refine_diff_density_min         -0.528
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     197
_refine_ls_number_reflns         4373
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0610
_refine_ls_R_factor_gt           0.0405
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0313P)²+5.5585P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0842
_refine_ls_wR_factor_ref         0.0953
_reflns_number_gt                3455
_reflns_number_total             4373
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2dt31678a.txt
_cod_data_source_block           compound
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7020485
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -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
Sn1 Sn 0.0000 0.457840(14) 0.2500 0.04265(10) Uani 1 2 d S
O1 O 0.1695(2) 0.53816(11) 0.24109(10) 0.0541(5) Uani 1 1 d .
N1 N -0.0345(3) 0.49684(12) 0.14779(10) 0.0410(5) Uani 1 1 d .
C8 C -0.1164(3) 0.45006(15) 0.10650(12) 0.0431(6) Uani 1 1 d .
C13 C -0.2718(4) 0.46226(17) 0.09671(14) 0.0505(7) Uani 1 1 d .
C7 C 0.0065(3) 0.56365(16) 0.13040(13) 0.0479(7) Uani 1 1 d .
H7 H -0.0212 0.5805 0.0922 0.057 Uiso 1 1 d R
C9 C -0.0377(4) 0.39228(17) 0.07715(14) 0.0517(7) Uani 1 1 d .
C6 C 0.0950(4) 0.62068(16) 0.16193(13) 0.0484(7) Uani 1 1 d .
C17 C -0.3645(4) 0.5175(2) 0.13306(16) 0.0624(9) Uani 1 1 d .
H17 H -0.2943 0.5454 0.1574 0.075 Uiso 1 1 d R
C12 C -0.3423(4) 0.4188(2) 0.05325(16) 0.0633(9) Uani 1 1 d .
H12 H -0.4475 0.4279 0.0444 0.076 Uiso 1 1 d R
C10 C -0.1155(4) 0.35011(19) 0.03497(16) 0.0615(9) Uani 1 1 d .
H10 H -0.0623 0.3099 0.0150 0.074 Uiso 1 1 d R
C14 C 0.1282(4) 0.3755(2) 0.08996(17) 0.0672(10) Uani 1 1 d .
H14 H 0.1626 0.4155 0.1158 0.081 Uiso 1 1 d R
C11 C -0.2648(4) 0.3644(2) 0.02226(16) 0.0663(9) Uani 1 1 d .
H11 H -0.3147 0.3359 -0.0082 0.080 Uiso 1 1 d R
C2 C 0.2620(4) 0.6649(2) 0.23875(17) 0.0719(11) Uani 1 1 d .
H2 H 0.3123 0.6573 0.2754 0.086 Uiso 1 1 d R
C1 C 0.1717(3) 0.60583(17) 0.21438(13) 0.0489(7) Uani 1 1 d .
C5 C 0.1098(5) 0.69394(19) 0.13638(17) 0.0717(10) Uani 1 1 d .
H5 H 0.0549 0.7056 0.1013 0.086 Uiso 1 1 d R
C15 C 0.1500(6) 0.2975(3) 0.1172(3) 0.141(2) Uani 1 1 d .
H15A H 0.2558 0.2887 0.1251 0.169 Uiso 1 1 d R
H15B H 0.1117 0.2576 0.0921 0.169 Uiso 1 1 d R
H15C H 0.0955 0.2966 0.1527 0.169 Uiso 1 1 d R
C4 C 0.1961(6) 0.7510(2) 0.1615(2) 0.0919(15) Uani 1 1 d .
H4 H 0.2051 0.8007 0.1432 0.110 Uiso 1 1 d R
C3 C 0.2713(6) 0.7360(2) 0.2126(2) 0.0930(15) Uani 1 1 d .
H3 H 0.3366 0.7753 0.2286 0.112 Uiso 1 1 d R
C18 C -0.4754(6) 0.4729(3) 0.1697(2) 0.1053(16) Uani 1 1 d .
H18A H -0.5334 0.5085 0.1922 0.126 Uiso 1 1 d R
H18B H -0.4197 0.4387 0.1950 0.126 Uiso 1 1 d R
H18C H -0.5425 0.4431 0.1454 0.126 Uiso 1 1 d R
C19 C -0.4500(6) 0.5772(3) 0.0980(2) 0.1107(18) Uani 1 1 d .
H19A H -0.5059 0.6106 0.1230 0.133 Uiso 1 1 d R
H19B H -0.5189 0.5512 0.0720 0.133 Uiso 1 1 d R
H19C H -0.3798 0.6075 0.0762 0.133 Uiso 1 1 d R
C16 C 0.2222(6) 0.3805(5) 0.0372(3) 0.155(3) Uani 1 1 d .
H16A H 0.3264 0.3698 0.0469 0.187 Uiso 1 1 d R
H16B H 0.2135 0.4319 0.0218 0.187 Uiso 1 1 d R
H16C H 0.1866 0.3438 0.0090 0.187 Uiso 1 1 d R
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_diffrn_radiation_wavelength
0.71073
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_1
_geom_angle_site_symmetry_3
O1 Sn1 O1 95.00(12) 2 .
O1 Sn1 N1 78.35(8) 2 2
O1 Sn1 N1 80.48(8) . 2
O1 Sn1 N1 80.48(8) 2 .
O1 Sn1 N1 78.35(8) . .
N1 Sn1 N1 148.45(10) 2 .
C1 O1 Sn1 131.33(19) . .
C7 N1 C8 116.1(2) . .
C7 N1 Sn1 121.14(18) . .
C8 N1 Sn1 122.44(16) . .
C9 C8 C13 121.4(3) . .
C9 C8 N1 118.5(3) . .
C13 C8 N1 120.1(3) . .
C12 C13 C8 117.3(3) . .
C12 C13 C17 120.0(3) . .
C8 C13 C17 122.6(3) . .
N1 C7 C6 127.5(3) . .
N1 C7 H7 119.7 . .
C6 C7 H7 112.8 . .
C10 C9 C8 118.2(3) . .
C10 C9 C14 120.0(3) . .
C8 C9 C14 121.8(3) . .
C5 C6 C1 118.8(3) . .
C5 C6 C7 117.0(3) . .
C1 C6 C7 124.1(3) . .
C19 C17 C18 109.2(4) . .
C19 C17 C13 113.5(3) . .
C18 C17 C13 110.5(3) . .
C19 C17 H17 106.6 . .
C18 C17 H17 109.9 . .
C13 C17 H17 107.0 . .
C11 C12 C13 121.8(3) . .
C11 C12 H12 119.3 . .
C13 C12 H12 118.9 . .
C11 C10 C9 121.3(3) . .
C11 C10 H10 120.2 . .
C9 C10 H10 118.5 . .
C16 C14 C15 109.2(5) . .
C16 C14 C9 112.1(4) . .
C15 C14 C9 111.8(3) . .
C16 C14 H14 107.1 . .
C15 C14 H14 110.3 . .
C9 C14 H14 106.1 . .
C10 C11 C12 119.8(3) . .
C10 C11 H11 119.6 . .
C12 C11 H11 120.5 . .
C3 C2 C1 120.6(4) . .
C3 C2 H2 119.0 . .
C1 C2 H2 120.3 . .
O1 C1 C6 123.7(3) . .
O1 C1 C2 117.7(3) . .
C6 C1 C2 118.5(3) . .
C4 C5 C6 121.7(4) . .
C4 C5 H5 118.5 . .
C6 C5 H5 119.8 . .
C14 C15 H15A 109.9 . .
C14 C15 H15B 110.3 . .
H15A C15 H15B 109.5 . .
C14 C15 H15C 108.2 . .
H15A C15 H15C 109.5 . .
H15B C15 H15C 109.5 . .
C5 C4 C3 119.2(4) . .
C5 C4 H4 120.3 . .
C3 C4 H4 120.5 . .
C2 C3 C4 121.3(3) . .
C2 C3 H3 120.1 . .
C4 C3 H3 118.5 . .
C17 C18 H18A 109.5 . .
C17 C18 H18B 109.0 . .
H18A C18 H18B 109.5 . .
C17 C18 H18C 109.9 . .
H18A C18 H18C 109.5 . .
H18B C18 H18C 109.5 . .
C17 C19 H19A 110.0 . .
C17 C19 H19B 108.9 . .
H19A C19 H19B 109.5 . .
C17 C19 H19C 109.6 . .
H19A C19 H19C 109.5 . .
H19B C19 H19C 109.4 . .
C14 C16 H16A 110.0 . .
C14 C16 H16B 108.4 . .
H16A C16 H16B 109.5 . .
C14 C16 H16C 109.9 . .
H16A C16 H16C 109.5 . .
H16B C16 H16C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Sn1 O1 2.0524(19) 2
Sn1 O1 2.0524(19) .
Sn1 N1 2.477(2) 2
Sn1 N1 2.477(2) .
O1 C1 1.323(3) .
N1 C7 1.276(3) .
N1 C8 1.438(3) .
C8 C9 1.398(4) .
C8 C13 1.402(4) .
C13 C12 1.394(4) .
C13 C17 1.520(5) .
C7 C6 1.447(4) .
C7 H7 0.9600 .
C9 C10 1.391(4) .
C9 C14 1.516(5) .
C6 C5 1.404(4) .
C6 C1 1.405(4) .
C17 C19 1.507(6) .
C17 C18 1.516(6) .
C17 H17 0.9601 .
C12 C11 1.372(5) .
C12 H12 0.9601 .
C10 C11 1.367(5) .
C10 H10 0.9599 .
C14 C16 1.491(6) .
C14 C15 1.497(6) .
C14 H14 0.9602 .
C11 H11 0.9601 .
C2 C3 1.371(5) .
C2 C1 1.407(4) .
C2 H2 0.9600 .
C5 C4 1.369(5) .
C5 H5 0.9601 .
C15 H15A 0.9600 .
C15 H15B 0.9599 .
C15 H15C 0.9599 .
C4 C3 1.373(6) .
C4 H4 0.9600 .
C3 H3 0.9600 .
C18 H18A 0.9600 .
C18 H18B 0.9601 .
C18 H18C 0.9598 .
C19 H19A 0.9600 .
C19 H19B 0.9601 .
C19 H19C 0.9602 .
C16 H16A 0.9600 .
C16 H16B 0.9600 .
C16 H16C 0.9601 .
