Unusual structural variations within a family of thioether macrocyclic complexes. Tin(iv) halide adducts of [12]-, [14]- and [16]-aneS4
Levason, William; Matthews, Melissa L.; Patel, Rina; Reid, Gillian; Webster, Michael; New Journal of Chemistry 27 (2003) 1784–; doi:10.1039/b307863a

data_7050667
_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_absolute_configuration unk
_chemical_formula_moiety         'C12 H24 Br4 S4 Sn'
_chemical_formula_sum            'C12 H24 Br4 S4 Sn'
_chemical_formula_weight         734.88
_chemical_name_common
1,5,9,13-tetrathiacyclohexadecane-tetrabromotin(IV)
_chemical_name_systematic
;
1,5,9,13-tetrathiacyclohexadecane-tetrabromotin(IV)
;
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      29
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_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                   19.4987(7)
_cell_length_b                   10.0624(3)
_cell_length_c                   10.9104(3)
_cell_measurement_reflns_used    16449
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.91
_cell_volume                     2140.66(12)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'area detector, Nonius Kappa ccd'
_diffrn_measurement_method       '\f and \w 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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0537
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            4590
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         2.91
_exptl_absorpt_coefficient_mu    9.042
_exptl_absorpt_correction_T_max  0.8916
_exptl_absorpt_correction_T_min  0.6117
_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    2.280
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1400
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.664
_refine_diff_density_min         -1.409
_refine_diff_density_rms         0.269
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.520(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     191
_refine_ls_number_reflns         4590
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0626
_refine_ls_R_factor_gt           0.0535
_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/[\s^2^(Fo^2^)+(0.0850P)^2^+7.0400P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1314
_refine_ls_wR_factor_ref         0.1380
_reflns_number_gt                4105
_reflns_number_total             4590
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b307863a.txt
_cod_data_source_block           '[SnBr4([16]aneS4)]'
_cod_database_code               7050667