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_7050666
_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         'C10 H20 Br4 S4 Sn, 0.67(C H2 Cl2)'
_chemical_formula_sum            'C10.67 H21.33 Br4 Cl1.33 S4 Sn'
_chemical_formula_weight         763.45
_chemical_name_common
;1,4,8,11-tetrathiacyclotetradecane-tetrabromotin(IV)
dichloromethane solvate
;
_chemical_name_systematic
;
1,4,8,11-tetrathiacyclotetradecane-tetrabromotin(IV) dichloromethane solvate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_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                104.8650(10)
_cell_angle_beta                 103.4750(10)
_cell_angle_gamma                92.8590(10)
_cell_formula_units_Z            3
_cell_length_a                   11.2865(3)
_cell_length_b                   11.5634(3)
_cell_length_c                   13.3067(4)
_cell_measurement_reflns_used    8678
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.91
_cell_volume                     1621.19(8)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.952
_diffrn_measured_fraction_theta_max 0.952
_diffrn_measurement_device_type  '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  0.0611
_diffrn_reflns_av_sigmaI/netI    0.0743
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            15354
_diffrn_reflns_theta_full        27.53
_diffrn_reflns_theta_max         27.53
_diffrn_reflns_theta_min         2.94
_exptl_absorpt_coefficient_mu    9.119
_exptl_absorpt_correction_T_max  0.62454
_exptl_absorpt_correction_T_min  0.53716
_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    2.346
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1086
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.06
_refine_diff_density_max         2.099
_refine_diff_density_min         -2.172
_refine_diff_density_rms         0.227
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     260
_refine_ls_number_reflns         7125
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0635
_refine_ls_R_factor_gt           0.0467
_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^)+(0.0263P)^2^+10.6581P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0997
_refine_ls_wR_factor_ref         0.1077
_reflns_number_gt                5762
_reflns_number_total             7125
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b307863a.txt
_cod_data_source_block           SnBr4([14]aneS4).2/3CH2Cl2
_cod_database_code               7050666