Novel Stannatranes of the Type N(CH2CMe2O)3SnX (X = OR, SR, OC(O)R, SP(S)Ph2, Halogen). Synthesis, Molecular Structures, and Electrochemical Properties
Thomas Zöller; Christina Dietz; Ljuba Iovkova-Berends; Olga Karsten; Gerrit Bradtmöller; Ann-Kristin Wiegand; Yu Wang; Viatcheslav Jouikov; Klaus Jurkschat; Inorganic Chemistry 51 (2012) 1041–1056; doi:10.1021/ic202179e

data_4328011
_publ_contact_author_address
;
    Lehrstuhl f\"ur Anorganische Chemie II
    Technische Universi\"at Dortmund
    44221 Dortmund
    Deutschland
;
_publ_contact_author_email       klaus.jurkschat@tu-dortmund.de
_publ_contact_author_name        'Klaus Jurkschat'
_publ_section_title
;
 Novel Stannatranes of the Type N(CH2CMe2O)3SnX (X = OR, SR, OC(O)R,
 SP(S)Ph2, Halogen). Synthesis, Molecular Structures, and Electrochemical
 Properties
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1041
_journal_page_last               1056
_journal_paper_doi               10.1021/ic202179e
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         'C19 H31 N O3 S Sn'
_chemical_formula_sum            'C19 H31 N O3 S Sn'
_chemical_formula_weight         472.20
_chemical_name_systematic
;
1-(4-Methylthiophenolato)-(2,8,9-trioxa-5-aza-3,3,7,7,10,10-hexamethyl-
stannatricyclo[3.3.3.01.5]undecane
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   15.6509(7)
_cell_length_b                   14.5103(9)
_cell_length_c                   18.3198(9)
_cell_measurement_reflns_used    4361
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      29.1903
_cell_measurement_theta_min      1.9132
_cell_volume                     4160.4(4)
_computing_cell_refinement
'CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55''
_computing_data_collection
'CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55''
_computing_data_reduction
'CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55''
_computing_molecular_graphics    'SHELXP-97 (Sheldrick, 1997)'
_computing_publication_material  'enCIFer Version 1.3'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       'Xcalibur2 CCD Diffractometer'
_diffrn_measurement_method       '\w und \y scan'
_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  0.0740
_diffrn_reflns_av_sigmaI/netI    0.1260
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            22760
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         2.21
_exptl_absorpt_coefficient_mu    1.345
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.77784
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.37 (release 24-10-2008 CrysAlis171 .NET)
(compiled Oct 24 2008,09:44:38)
empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.508
_exptl_crystal_description       column
_exptl_crystal_F_000             1936
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.409
_refine_diff_density_min         -0.438
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.631
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     227
_refine_ls_number_reflns         4514
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.631
_refine_ls_R_factor_all          0.0878
_refine_ls_R_factor_gt           0.0256
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0100P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0357
_refine_ls_wR_factor_ref         0.0387
_reflns_number_gt                2034
_reflns_number_total             4514
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic202179e_si_001_07.cif
_cod_data_source_block           0972t
_cod_database_code               4328011