#------------------------------------------------------------------------------
#$Date: 2019-03-05 10:52:05 +0200 (Tue, 05 Mar 2019) $
#$Revision: 213973 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/05/06/7050665.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_7050665
loop_
_publ_author_name
'Levason, William'
'Matthews, Melissa L.'
'Patel, Rina'
'Reid, Gillian'
'Webster, Michael'
_publ_section_title
;
 Unusual structural variations within a family of thioether macrocyclic
 complexes. Tin(iv) halide adducts of [12]-, [14]- and [16]-aneS4
;
_journal_issue                   12
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              1784
_journal_paper_doi               10.1039/b307863a
_journal_volume                  27
_journal_year                    2003
_chemical_formula_moiety         'C8 H16 Br4 S4 Sn'
_chemical_formula_sum            'C8 H16 Br4 S4 Sn'
_chemical_formula_weight         678.78
_chemical_name_common
1,4,7,10-tetrathiacyclododecane-tetrabromotin(IV)
_chemical_name_systematic
;
1,4,7,10-tetrathiacyclododecane-tetrabromotin(IV)
;
_space_group_IT_number           63
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      63
_symmetry_space_group_name_Hall  '-C 2c 2'
_symmetry_space_group_name_H-M   'C m c m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'SHELXL-97 + hand edit'
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.5135(3)
_cell_length_b                   8.3306(3)
_cell_length_c                   19.6638(7)
_cell_measurement_reflns_used    6593
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.91
_cell_volume                     1722.23(10)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Nonius rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0983
_diffrn_reflns_av_sigmaI/netI    0.0530
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            5824
_diffrn_reflns_theta_full        27.45
_diffrn_reflns_theta_max         27.45
_diffrn_reflns_theta_min         3.12
_exptl_absorpt_coefficient_mu    11.227
_exptl_absorpt_correction_T_max  0.20894
_exptl_absorpt_correction_T_min  0.07609
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SORTAV, R H Blessing, J. Appl. Cryst., 1997, 30, 421-426.'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    2.618
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1272
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.393
_refine_diff_density_min         -2.487
_refine_diff_density_rms         0.277
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     46
_refine_ls_number_reflns         1069
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0447
_refine_ls_R_factor_gt           0.0412
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0684P)²+6.010P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1046
_refine_ls_wR_factor_ref         0.1072
_reflns_number_gt                991
_reflns_number_total             1069
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b307863a.txt
_cod_data_source_block           '[SnBr4([12]aneS4)]'
_cod_database_code               7050665
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'-x, y, -z+1/2'
'x, -y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x, y, -z-1/2'
'x, -y, z-1/2'
'-x, y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, y+1/2, -z-1/2'
'x+1/2, -y+1/2, z-1/2'
'-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_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Sn1 Sn 0.0000 0.17621(7) 0.2500 0.0140(2) Uani 1 4 d S . .
Br1 Br 0.24264(6) 0.19916(8) 0.2500 0.0174(2) Uani 1 2 d S . .
Br2 Br 0.0000 -0.01554(8) 0.14952(3) 0.0199(2) Uani 1 2 d S . .
S1 S 0.28824(16) 0.5000 0.0000 0.0197(4) Uani 1 2 d S . .
S2 S 0.0000 0.4363(2) 0.16227(7) 0.0159(3) Uani 1 2 d S . .
C1 C 0.1333(5) 0.4001(7) 0.1045(2) 0.0203(10) Uani 1 1 d . . .
H1A H 0.2061 0.3579 0.1309 0.024 Uiso 1 1 calc R . .
H1B H 0.1083 0.3169 0.0711 0.024 Uiso 1 1 calc R . .
C2 C 0.1756(5) 0.5496(6) 0.0663(2) 0.0198(9) Uani 1 1 d . . .
H2A H 0.2153 0.6258 0.0986 0.024 Uiso 1 1 calc R . .
H2B H 0.1005 0.6027 0.0460 0.024 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Sn1 0.0138(3) 0.0175(4) 0.0108(3) 0.000 0.000 0.000
Br1 0.0145(4) 0.0245(4) 0.0133(3) 0.000 0.000 0.0002(2)
Br2 0.0200(4) 0.0228(4) 0.0167(3) -0.0057(2) 0.000 0.000
S1 0.0157(8) 0.0305(9) 0.0128(7) 0.0029(6) 0.000 0.000
S2 0.0170(8) 0.0192(8) 0.0115(6) 0.0009(5) 0.000 0.000
C1 0.024(2) 0.023(2) 0.015(2) 0.0044(17) 0.0041(16) 0.002(2)
C2 0.023(2) 0.023(2) 0.0136(19) -0.0026(17) 0.0032(17) -0.002(2)
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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 '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
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Br2 Sn1 Br2 102.09(4) . 10_556 ?
Br2 Sn1 Br1 92.693(13) . . ?
Br2 Sn1 Br1 92.693(13) 10_556 . ?
Br2 Sn1 Br1 92.693(13) . 3 ?
Br2 Sn1 Br1 92.693(13) 10_556 3 ?
Br1 Sn1 Br1 171.43(4) . 3 ?
Br2 Sn1 S2 167.48(4) . 10_556 ?
Br2 Sn1 S2 90.43(3) 10_556 10_556 ?
Br1 Sn1 S2 86.648(17) . 10_556 ?
Br1 Sn1 S2 86.648(17) 3 10_556 ?
Br2 Sn1 S2 90.43(3) . . ?
Br2 Sn1 S2 167.48(4) 10_556 . ?
Br1 Sn1 S2 86.648(17) . . ?
Br1 Sn1 S2 86.648(17) 3 . ?
S2 Sn1 S2 77.05(7) 10_556 . ?
C2 S1 C2 98.2(3) 4_565 . ?
C1 S2 C1 100.0(3) 12 . ?
C1 S2 Sn1 104.95(17) 12 . ?
C1 S2 Sn1 104.95(17) . . ?
C2 C1 S2 113.3(4) . . ?
C2 C1 H1A 108.9 . . ?
S2 C1 H1A 108.9 . . ?
C2 C1 H1B 108.9 . . ?
S2 C1 H1B 108.9 . . ?
H1A C1 H1B 107.7 . . ?
C1 C2 S1 111.1(3) . . ?
C1 C2 H2A 109.4 . . ?
S1 C2 H2A 109.4 . . ?
C1 C2 H2B 109.4 . . ?
S1 C2 H2B 109.4 . . ?
H2A C2 H2B 108.0 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Sn1 Br2 2.5407(7) . ?
Sn1 Br2 2.5407(7) 10_556 ?
Sn1 Br1 2.5582(7) . ?
Sn1 Br1 2.5582(7) 3 ?
Sn1 S2 2.7697(17) 10_556 ?
Sn1 S2 2.7697(17) . ?
S1 C2 1.810(5) 4_565 ?
S1 C2 1.810(5) . ?
S2 C1 1.829(5) 12 ?
S2 C1 1.829(5) . ?
C1 C2 1.520(7) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 H2A 0.9900 . ?
C2 H2B 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_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Br2 Sn1 S2 C1 52.46(18) . . . 12 ?
Br2 Sn1 S2 C1 -127.54(18) 10_556 . . 12 ?
Br1 Sn1 S2 C1 145.13(18) . . . 12 ?
Br1 Sn1 S2 C1 -40.22(18) 3 . . 12 ?
S2 Sn1 S2 C1 -127.54(18) 10_556 . . 12 ?
Br2 Sn1 S2 C1 -52.46(18) . . . . ?
Br2 Sn1 S2 C1 127.54(18) 10_556 . . . ?
Br1 Sn1 S2 C1 40.22(18) . . . . ?
Br1 Sn1 S2 C1 -145.13(18) 3 . . . ?
S2 Sn1 S2 C1 127.54(18) 10_556 . . . ?
C1 S2 C1 C2 89.0(4) 12 . . . ?
Sn1 S2 C1 C2 -162.5(3) . . . . ?
S2 C1 C2 S1 -170.2(3) . . . . ?
C2 S1 C2 C1 85.4(3) 4_565 . . . ?
