#------------------------------------------------------------------------------
#$Date: 2016-02-13 14:50:18 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176428 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/47/7034777.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_7034777
loop_
_publ_author_name
'Mansell, S. M.'
'Russell, C. A.'
'Wass, D. F.'
_publ_section_title
;
 Synthesis of chelating diamido Sn(iv) compounds from oxidation of Sn(ii)
 and directly from Sn(iv) precursors.
;
_journal_issue                   21
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9756
_journal_page_last               9765
_journal_paper_doi               10.1039/c5dt01022e
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C27 H40 Cl2 N2 Sn'
_chemical_formula_sum            'C27 H40 Cl2 N2 Sn'
_chemical_formula_weight         582.22
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2014-10-03 deposited with the CCDC.
2015-04-21 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.053(2)
_cell_length_b                   22.006(4)
_cell_length_c                   10.470(2)
_cell_measurement_reflns_used    8390
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.472
_cell_measurement_theta_min      2.154
_cell_volume                     2777.0(9)
_computing_cell_refinement       'BRUKER SAINT'
_computing_data_collection       'BRUKER SMART'
_computing_data_reduction        'BRUKER SAINT'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.5
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'omega 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  0.0265
_diffrn_reflns_av_sigmaI/netI    0.0192
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            18836
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.58
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.129
_exptl_absorpt_correction_T_max  0.64
_exptl_absorpt_correction_T_min  0.47065
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2.10 (BRUKER-AXS, 2003)'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.392
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1200
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.761
_refine_diff_density_min         -0.457
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.432
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     155
_refine_ls_number_reflns         3274
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.432
_refine_ls_R_factor_all          0.0259
_refine_ls_R_factor_gt           0.0235
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0262P)²+0.1727P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0600
_refine_ls_wR_factor_ref         0.0607
_reflns_number_gt                3083
_reflns_number_total             3274
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5dt01022e2.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 7034774--7034789.cif.'
_cod_original_cell_volume        2777.2(10)
_cod_original_sg_symbol_H-M      'P nma'
_cod_database_code               7034777
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -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 0.866986(12) 0.7500 0.843572(14) 0.01181(6) Uani 1 2 d S
Cl1 Cl 0.67893(5) 0.7500 0.88408(6) 0.02106(14) Uani 1 2 d S
Cl2 Cl 0.86702(5) 0.7500 0.62010(6) 0.02195(14) Uani 1 2 d S
N1 N 0.94471(11) 0.68103(6) 0.92596(13) 0.0133(3) Uani 1 1 d .
C1 C 0.90531(13) 0.61977(7) 0.92978(15) 0.0126(3) Uani 1 1 d .
C2 C 0.84231(13) 0.60116(8) 1.03630(15) 0.0136(3) Uani 1 1 d .
C3 C 0.81106(14) 0.54038(8) 1.04463(15) 0.0167(3) Uani 1 1 d .
H3 H 0.7683 0.5271 1.1156 0.020 Uiso 1 1 calc R
C4 C 0.84102(14) 0.49901(8) 0.95165(17) 0.0185(4) Uani 1 1 d .
H4 H 0.8204 0.4575 0.9601 0.022 Uiso 1 1 calc R
C5 C 0.90104(16) 0.51788(8) 0.84631(15) 0.0180(4) Uani 1 1 d .
H5 H 0.9210 0.4891 0.7827 0.022 Uiso 1 1 calc R
C6 C 0.93279(14) 0.57853(8) 0.83196(15) 0.0143(3) Uani 1 1 d .
C7 C 0.81030(15) 0.64510(8) 1.14204(15) 0.0177(4) Uani 1 1 d .
H7 H 0.8300 0.6870 1.1128 0.021 Uiso 1 1 calc R
C8 C 0.87663(16) 0.63214(12) 1.26410(19) 0.0348(6) Uani 1 1 d .
H8A H 0.8565 0.6618 1.3300 0.052 Uiso 1 1 calc R
H8B H 0.9562 0.6353 1.2457 0.052 Uiso 1 1 calc R
H8C H 0.8596 0.5911 1.2946 0.052 Uiso 1 1 calc R
C9 C 0.68617(16) 0.64436(10) 1.17026(17) 0.0261(4) Uani 1 1 d .
H9A H 0.6449 0.6527 1.0916 0.039 Uiso 1 1 calc R
H9B H 0.6689 0.6756 1.2340 0.039 Uiso 1 1 calc R
H9C H 0.6650 0.6043 1.2034 0.039 Uiso 1 1 calc R
C10 C 0.99741(14) 0.59804(8) 0.71412(15) 0.0164(3) Uani 1 1 d .
H10 H 1.0040 0.6433 0.7162 0.020 Uiso 1 1 calc R
C11 C 1.11512(15) 0.57160(10) 0.71420(19) 0.0262(4) Uani 1 1 d .
H11A H 1.1526 0.5826 0.7940 0.039 Uiso 1 1 calc R
H11B H 1.1568 0.5881 0.6417 0.039 Uiso 1 1 calc R
H11C H 1.1112 0.5273 0.7069 0.039 Uiso 1 1 calc R
C12 C 0.93691(17) 0.58081(10) 0.59110(16) 0.0287(4) Uani 1 1 d .
H12A H 0.9322 0.5365 0.5846 0.043 Uiso 1 1 calc R
H12B H 0.9778 0.5968 0.5175 0.043 Uiso 1 1 calc R
H12C H 0.8620 0.5981 0.5922 0.043 Uiso 1 1 calc R
C13 C 1.06143(14) 0.69132(8) 0.96301(18) 0.0208(4) Uani 1 1 d .
H13A H 1.1078 0.6910 0.8850 0.025 Uiso 1 1 calc R
H13B H 1.0860 0.6571 1.0176 0.025 Uiso 1 1 calc R
C14 C 1.0815(2) 0.7500 1.0335(3) 0.0234(6) Uani 1 2 d S
H14A H 1.0338 0.7500 1.1105 0.028 Uiso 1 2 calc SR
H14B H 1.1594 0.7500 1.0632 0.028 Uiso 1 2 calc SR
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'
Cl Cl 0.1484 0.1585 '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_
_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
N1 Sn1 N1 100.00(8) 7_575
N1 Sn1 Cl1 112.62(4) 7_575
N1 Sn1 Cl1 112.62(4) .
N1 Sn1 Cl2 115.81(4) 7_575
N1 Sn1 Cl2 115.80(4) .
Cl1 Sn1 Cl2 100.61(2) .
C1 N1 C13 116.97(13) .
C1 N1 Sn1 125.27(10) .
C13 N1 Sn1 116.58(10) .
C6 C1 C2 120.99(15) .
C6 C1 N1 120.61(15) .
C2 C1 N1 118.34(14) .
C3 C2 C1 118.31(15) .
C3 C2 C7 119.79(15) .
C1 C2 C7 121.89(15) .
C4 C3 C2 121.22(16) .
C4 C3 H3 119.4 .
C2 C3 H3 119.4 .
C3 C4 C5 120.08(16) .
C3 C4 H4 120.0 .
C5 C4 H4 120.0 .
C4 C5 C6 121.07(16) .
C4 C5 H5 119.5 .
C6 C5 H5 119.5 .
C5 C6 C1 118.25(15) .
C5 C6 C10 119.83(15) .
C1 C6 C10 121.91(15) .
C2 C7 C9 112.55(15) .
C2 C7 C8 110.88(16) .
C9 C7 C8 110.35(15) .
C2 C7 H7 107.6 .
C9 C7 H7 107.6 .
C8 C7 H7 107.6 .
C7 C8 H8A 109.5 .
C7 C8 H8B 109.5 .
H8A C8 H8B 109.5 .
C7 C8 H8C 109.5 .
H8A C8 H8C 109.5 .
H8B C8 H8C 109.5 .
C7 C9 H9A 109.5 .
C7 C9 H9B 109.5 .
H9A C9 H9B 109.5 .
C7 C9 H9C 109.5 .
H9A C9 H9C 109.5 .
H9B C9 H9C 109.5 .
C6 C10 C12 111.67(15) .
C6 C10 C11 111.48(14) .
C12 C10 C11 110.35(15) .
C6 C10 H10 107.7 .
C12 C10 H10 107.7 .
C11 C10 H10 107.7 .
C10 C11 H11A 109.5 .
C10 C11 H11B 109.5 .
H11A C11 H11B 109.5 .
C10 C11 H11C 109.5 .
H11A C11 H11C 109.5 .
H11B C11 H11C 109.5 .
C10 C12 H12A 109.5 .
C10 C12 H12B 109.5 .
H12A C12 H12B 109.5 .
C10 C12 H12C 109.5 .
H12A C12 H12C 109.5 .
H12B C12 H12C 109.5 .
N1 C13 C14 114.37(16) .
N1 C13 H13A 108.7 .
C14 C13 H13A 108.7 .
N1 C13 H13B 108.7 .
C14 C13 H13B 108.7 .
H13A C13 H13B 107.6 .
C13 C14 C13 118.0(2) 7_575
C13 C14 H14A 107.8 7_575
C13 C14 H14A 107.8 .
C13 C14 H14B 107.8 7_575
C13 C14 H14B 107.8 .
H14A C14 H14B 107.1 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Sn1 N1 1.9811(13) 7_575
Sn1 N1 1.9812(13) .
Sn1 Cl1 2.3059(8) .
Sn1 Cl2 2.3398(8) .
N1 C1 1.430(2) .
N1 C13 1.477(2) .
C1 C6 1.408(2) .
C1 C2 1.410(2) .
C2 C3 1.392(2) .
C2 C7 1.520(2) .
C3 C4 1.381(2) .
C3 H3 0.9500 .
C4 C5 1.383(3) .
C4 H4 0.9500 .
C5 C6 1.397(2) .
C5 H5 0.9500 .
C6 C10 1.521(2) .
C7 C9 1.525(3) .
C7 C8 1.534(2) .
C7 H7 1.0000 .
C8 H8A 0.9800 .
C8 H8B 0.9800 .
C8 H8C 0.9800 .
C9 H9A 0.9800 .
C9 H9B 0.9800 .
C9 H9C 0.9800 .
C10 C12 1.528(2) .
C10 C11 1.533(2) .
C10 H10 1.0000 .
C11 H11A 0.9800 .
C11 H11B 0.9800 .
C11 H11C 0.9800 .
C12 H12A 0.9800 .
C12 H12B 0.9800 .
C12 H12C 0.9800 .
C13 C14 1.507(2) .
C13 H13A 0.9900 .
C13 H13B 0.9900 .
C14 C13 1.507(2) 7_575
C14 H14A 0.9900 .
C14 H14B 0.9900 .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
N1 Sn1 N1 C1 162.50(10) 7_575 .
Cl1 Sn1 N1 C1 42.72(14) . .
Cl2 Sn1 N1 C1 -72.31(13) . .
N1 Sn1 N1 C13 -30.36(15) 7_575 .
Cl1 Sn1 N1 C13 -150.14(11) . .
Cl2 Sn1 N1 C13 94.83(12) . .
C13 N1 C1 C6 -77.6(2) . .
Sn1 N1 C1 C6 89.53(17) . .
C13 N1 C1 C2 99.87(18) . .
Sn1 N1 C1 C2 -93.04(16) . .
C6 C1 C2 C3 2.2(2) . .
N1 C1 C2 C3 -175.26(14) . .
C6 C1 C2 C7 -179.11(15) . .
N1 C1 C2 C7 3.5(2) . .
C1 C2 C3 C4 0.3(2) . .
C7 C2 C3 C4 -178.48(15) . .
C2 C3 C4 C5 -1.5(3) . .
C3 C4 C5 C6 0.3(3) . .
C4 C5 C6 C1 2.1(3) . .
C4 C5 C6 C10 -179.17(16) . .
C2 C1 C6 C5 -3.3(2) . .
N1 C1 C6 C5 174.05(15) . .
C2 C1 C6 C10 177.97(15) . .
N1 C1 C6 C10 -4.7(2) . .
C3 C2 C7 C9 -53.4(2) . .
C1 C2 C7 C9 127.93(17) . .
C3 C2 C7 C8 70.8(2) . .
C1 C2 C7 C8 -107.91(19) . .
C5 C6 C10 C12 55.1(2) . .
C1 C6 C10 C12 -126.19(17) . .
C5 C6 C10 C11 -68.8(2) . .
C1 C6 C10 C11 109.86(19) . .
C1 N1 C13 C14 -144.44(17) . .
Sn1 N1 C13 C14 47.3(2) . .
N1 C13 C14 C13 -64.7(3) . 7_575
