#------------------------------------------------------------------------------
#$Date: 2011-09-10 04:16:28 +0100 (Sat, 10 Sep 2011) $
#$Revision: 25271 $
#$URL: svn://www.crystallography.net/cod/cif/2/2011458.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2011458
loop_
_publ_author_name
'K\"onig, Uwe-Christoph'
'Berkei, Michael'
'Hirsch, Claudia'
'Preut, Hans'
'Mitchell, Terence Nigel'
_publ_section_title
;
 <i>cis</i>-Dibromo-<i>trans</i>-dimethyl-<i>cis</i>-bis(<i>N</i>,<i>N</i>-dimethylacetamide)tin(IV)
;
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              e452
_journal_page_last               e453
_journal_volume                  56
_journal_year                    2000
_chemical_formula_iupac          '[Sn Br2 (C H3)2 (C4 H9 N O)2]'
_chemical_formula_sum            'C10 H24 Br2 N2 O2 Sn'
_chemical_formula_weight         482.83
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 107.42(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.798(3)
_cell_length_b                   9.3350(19)
_cell_length_c                   13.729(3)
_cell_measurement_reflns_used    4990
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.01
_cell_measurement_theta_min      2.85
_cell_volume                     1687.3(7)
_computing_cell_refinement
;
DENZO and SCALEPACK (Otwinowski & Minor, 1997)
;
_computing_data_collection       'KappaCCD Software (Nonius, 1998)'
_computing_data_reduction
;
DENZO and SCALEPACK
;
_computing_publication_material  'SHELXL97 and PARST95 (Nardelli, 1995)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean '10 vertical, 18 horizontal'
_diffrn_measured_fraction_theta_full .893
_diffrn_measured_fraction_theta_max .893
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method
;
294 frames via \w rotation (\D\w = 1\%) at different \k
values and two times 80 s per frame
;
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .022
_diffrn_reflns_av_sigmaI/netI    .0523
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            4990
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         2.85
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.245
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.901
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             936
_exptl_crystal_size_max          .14
_exptl_crystal_size_mid          .13
_exptl_crystal_size_min          .13
_refine_diff_density_max         1.333
_refine_diff_density_min         -1.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     162
_refine_ls_number_reflns         2849
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          .043
_refine_ls_R_factor_gt           .033
_refine_ls_shift/su_max          <0.001
_refine_ls_shift/su_mean         <0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
'calc w = 1/[\s^2^(Fo^2^)+(0.0276P)^2^+1.0314P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_wR_factor_ref         .078
_reflns_number_gt                2307
_reflns_number_total             2849
_reflns_threshold_expression     I>2\s(I)
_[local]_cod_data_source_file    qa0387.cif
_[local]_cod_data_source_block   I
_[local]_cod_cif_authors_sg_H-M  'P 21/c'
_cod_original_cell_volume        1687.3(6)
_cod_database_code               2011458
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_type_symbol
Sn1 .25081(2) .11729(3) .06699(2) .02993(13) Uani d . 1 Sn
Br1 .11096(4) .24649(6) .13359(4) .04875(18) Uani d . 1 Br
O1 .3783(2) -.0032(4) .0182(3) .0422(8) Uani d . 1 O
C1 .3659(3) .1436(5) .2067(4) .0401(13) Uani d . 1 C
H1A .3376 .1321 .2621 .060 Uiso calc R 1 H
H1B .3948 .2377 .2095 .060 Uiso calc R 1 H
H1C .4179 .0731 .2121 .060 Uiso calc R 1 H
N1 .4003(4) -.2093(8) -.0510(7) .114(3) Uani d . 1 N
Br2 .29303(4) .34828(5) -.02339(4) .04081(16) Uani d . 1 Br
O2 .2289(2) -.1078(3) .1419(2) .0390(8) Uani d . 1 O
C2 .1445(3) .0304(6) -.0644(4) .0449(13) Uani d . 1 C
H2A .1664 -.0632 -.0777 .067 Uiso calc R 1 H
H2B .1395 .0916 -.1219 .067 Uiso calc R 1 H
H2C .0792 .0235 -.0532 .067 Uiso calc R 1 H
N2 .1149(4) -.2757(7) .1400(5) .095(2) Uani d . 1 N
C11 .3802(4) -.0921(8) -.0479(7) .081(3) Uani d . 1 C
C12 .3473(4) -.0276(7) -.1691(5) .0632(17) Uani d . 1 C
H12A .4037 -.0374 -.1960 .095 Uiso calc R 1 H
H12B .3292 .0717 -.1689 .095 Uiso calc R 1 H
H12C .2904 -.0807 -.2109 .095 Uiso calc R 1 H
C13 .4375(4) -.2673(7) .0659(4) .0592(17) Uani d . 1 C
H13A .5103 -.2738 .0887 .089 Uiso calc R 1 H
H13B .4088 -.3602 .0691 .089 Uiso calc R 1 H
H13C .4154 -.2021 .1090 .089 Uiso calc R 1 H
C14 .4113(4) -.3119(6) -.1266(4) .0483(14) Uani d . 1 C
H14A .3865 -.2704 -.1934 .072 Uiso calc R 1 H
H14B .3731 -.3967 -.1233 .072 Uiso calc R 1 H
H14C .4817 -.3363 -.1129 .072 Uiso calc R 1 H
C21 .1598(5) -.1739(8) .1653(7) .094(3) Uani d . 1 C
C22 .1237(4) -.1084(6) .2614(4) .0483(14) Uani d . 1 C
H22A .0513 -.0966 .2401 .072 Uiso calc R 1 H
H22B .1558 -.0173 .2815 .072 Uiso calc R 1 H
H22C .1433 -.1734 .3181 .072 Uiso calc R 1 H
C23 .0355(4) -.3579(5) .1615(4) .0443(13) Uani d . 1 C
H23A .0175 -.3147 .2172 .066 Uiso calc R 1 H
H23B .0590 -.4539 .1797 .066 Uiso calc R 1 H
H23C -.0229 -.3600 .1021 .066 Uiso calc R 1 H
C24 .1525(5) -.3455(6) .0460(4) .0560(16) Uani d . 1 C
H24A .0976 -.3417 -.0165 .084 Uiso calc R 1 H
H24B .1726 -.4433 .0618 .084 Uiso calc R 1 H
H24C .2091 -.2918 .0383 .084 Uiso calc R 1 H
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Sn1 .0284(2) .0303(2) .0308(2) -.00073(13) .00845(14) -.00065(14)
Br1 .0469(3) .0491(4) .0592(4) .0127(3) .0294(3) .0090(3)
O1 .0372(19) .039(2) .051(2) .0032(16) .0138(16) -.0110(17)
C1 .035(3) .046(3) .035(3) -.008(2) .005(2) -.004(2)
N1 .055(4) .097(5) .209(9) -.037(4) .068(4) -.105(6)
Br2 .0465(3) .0350(3) .0461(3) .0018(2) .0218(3) .0078(2)
O2 .038(2) .034(2) .045(2) -.0086(16) .0137(16) .0033(16)
C2 .036(3) .047(3) .046(3) -.008(2) .004(2) -.006(3)
N2 .044(3) .094(5) .130(6) -.009(3) .002(3) .078(4)
C11 .042(4) .053(5) .161(8) -.025(3) .049(4) -.047(5)
C12 .061(4) .065(4) .061(4) .002(3) .014(3) .029(3)
C13 .059(4) .088(5) .028(3) .010(3) .009(3) .012(3)
C14 .046(3) .041(3) .060(4) -.005(3) .019(3) -.017(3)
C21 .048(4) .061(5) .134(7) -.011(4) -.033(4) .065(5)
C22 .057(3) .056(4) .036(3) .010(3) .021(3) -.015(3)
C23 .041(3) .039(3) .055(4) -.009(2) .019(3) .001(3)
C24 .068(4) .061(4) .043(3) .017(3) .021(3) -.019(3)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O .0106 .0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sn Sn -.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_publ_flag
C1 Sn1 C2 164.2(2) y
C1 Sn1 O1 83.70(16) y
C2 Sn1 O1 87.75(16) y
C1 Sn1 O2 82.48(16) y
C2 Sn1 O2 83.44(16) y
O1 Sn1 O2 84.46(11) y
C1 Sn1 Br2 96.91(14) y
C2 Sn1 Br2 96.12(14) y
O1 Sn1 Br2 88.15(9) y
O2 Sn1 Br2 172.61(8) y
C1 Sn1 Br1 93.51(14) y
C2 Sn1 Br1 94.45(14) y
O1 Sn1 Br1 176.46(9) y
O2 Sn1 Br1 93.02(8) y
Br2 Sn1 Br1 94.37(2) y
C11 O1 Sn1 135.5(3) ?
Sn1 C1 H1A 109.5 ?
Sn1 C1 H1B 109.5 ?
H1A C1 H1B 109.5 ?
Sn1 C1 H1C 109.5 ?
H1A C1 H1C 109.5 ?
H1B C1 H1C 109.5 ?
C11 N1 C14 137.9(10) ?
C11 N1 C13 107.1(7) ?
C14 N1 C13 114.6(6) ?
C21 O2 Sn1 137.9(4) ?
Sn1 C2 H2A 109.5 ?
Sn1 C2 H2B 109.5 ?
H2A C2 H2B 109.5 ?
Sn1 C2 H2C 109.5 ?
H2A C2 H2C 109.5 ?
H2B C2 H2C 109.5 ?
C21 N2 C23 140.0(9) ?
C21 N2 C24 107.4(7) ?
C23 N2 C24 112.6(6) ?
N1 C11 O1 137.3(10) ?
N1 C11 C12 107.6(8) ?
O1 C11 C12 115.0(6) ?
C11 C12 H12A 109.5 ?
C11 C12 H12B 109.5 ?
H12A C12 H12B 109.5 ?
C11 C12 H12C 109.5 ?
H12A C12 H12C 109.5 ?
H12B C12 H12C 109.5 ?
N1 C13 H13A 109.5 ?
N1 C13 H13B 109.5 ?
H13A C13 H13B 109.5 ?
N1 C13 H13C 109.5 ?
H13A C13 H13C 109.5 ?
H13B C13 H13C 109.5 ?
N1 C14 H14A 109.5 ?
N1 C14 H14B 109.5 ?
H14A C14 H14B 109.5 ?
N1 C14 H14C 109.5 ?
H14A C14 H14C 109.5 ?
H14B C14 H14C 109.5 ?
N2 C21 O2 136.3(11) ?
N2 C21 C22 106.7(8) ?
O2 C21 C22 117.0(7) ?
C21 C22 H22A 109.5 ?
C21 C22 H22B 109.5 ?
H22A C22 H22B 109.5 ?
C21 C22 H22C 109.5 ?
H22A C22 H22C 109.5 ?
H22B C22 H22C 109.5 ?
N2 C23 H23A 109.5 ?
N2 C23 H23B 109.5 ?
H23A C23 H23B 109.5 ?
N2 C23 H23C 109.5 ?
H23A C23 H23C 109.5 ?
H23B C23 H23C 109.5 ?
N2 C24 H24A 109.5 ?
N2 C24 H24B 109.5 ?
H24A C24 H24B 109.5 ?
N2 C24 H24C 109.5 ?
H24A C24 H24C 109.5 ?
H24B C24 H24C 109.5 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Sn1 C1 2.107(4) y
Sn1 C2 2.117(5) y
Sn1 O1 2.348(3) y
Sn1 O2 2.398(3) y
Sn1 Br2 2.6385(7) y
Sn1 Br1 2.6589(8) y
O1 C11 1.236(8) ?
C1 H1A .9600 ?
C1 H1B .9600 ?
C1 H1C .9600 ?
N1 C11 1.133(8) ?
N1 C14 1.453(7) ?
N1 C13 1.624(10) ?
O2 C21 1.256(8) ?
C2 H2A .9600 ?
C2 H2B .9600 ?
C2 H2C .9600 ?
N2 C21 1.130(8) ?
N2 C23 1.439(7) ?
N2 C24 1.662(9) ?
C11 C12 1.698(10) ?
C12 H12A .9600 ?
C12 H12B .9600 ?
C12 H12C .9600 ?
C13 H13A .9600 ?
C13 H13B .9600 ?
C13 H13C .9600 ?
C14 H14A .9600 ?
C14 H14B .9600 ?
C14 H14C .9600 ?
C21 C22 1.659(11) ?
C22 H22A .9600 ?
C22 H22B .9600 ?
C22 H22C .9600 ?
C23 H23A .9600 ?
C23 H23B .9600 ?
C23 H23C .9600 ?
C24 H24A .9600 ?
C24 H24B .9600 ?
C24 H24C .9600 ?
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
C1 Sn1 O1 C11 158.8(7)
C2 Sn1 O1 C11 -7.8(7)
O2 Sn1 O1 C11 75.8(7)
Br2 Sn1 O1 C11 -104.0(7)
Br1 Sn1 O1 C11 120.6(13)
C1 Sn1 O2 C21 121.4(7)
C2 Sn1 O2 C21 -65.9(7)
O1 Sn1 O2 C21 -154.3(7)
Br2 Sn1 O2 C21 -152.9(7)
Br1 Sn1 O2 C21 28.2(7)
C14 N1 C11 O1 -173.2(6)
C13 N1 C11 O1 -1.2(10)
C14 N1 C11 C12 5.0(10)
C13 N1 C11 C12 176.9(4)
Sn1 O1 C11 N1 -109.9(9)
Sn1 O1 C11 C12 72.0(7)
C23 N2 C21 O2 -179.6(6)
C24 N2 C21 O2 -2.2(10)
C23 N2 C21 C22 4.3(10)
C24 N2 C21 C22 -178.3(4)
Sn1 O2 C21 N2 115.1(8)
Sn1 O2 C21 C22 -69.1(7)