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_4328010
_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         'C30 H38 N O4 P Sn'
_chemical_formula_sum            'C30 H38 N O4 P Sn'
_chemical_formula_weight         626.27
_chemical_name_systematic
;
1-(4-Diphenylphosphinophenolato)-(2,8,9-trioxa-5-aza-3,3,7,7,10,10-hexamethyl-
stannatricyclo[3.3.3.01.5]undecane
;
_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'
_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                 104.335(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.3731(11)
_cell_length_b                   12.6262(7)
_cell_length_c                   16.0139(9)
_cell_measurement_reflns_used    4782
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      29.0657
_cell_measurement_theta_min      2.1893
_cell_volume                     2815.7(3)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0624
_diffrn_reflns_av_sigmaI/netI    0.1293
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            14122
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         2.35
_exptl_absorpt_coefficient_mu    1.000
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91833
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan  5 2010,16:28:46)
empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.477
_exptl_crystal_description       plate
_exptl_crystal_F_000             1288
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.542
_refine_diff_density_min         -0.526
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.724
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         5250
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.724
_refine_ls_R_factor_all          0.0725
_refine_ls_R_factor_gt           0.0329
_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^)+(0.0109P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0448
_refine_ls_wR_factor_ref         0.0477
_reflns_number_gt                3118
_reflns_number_total             5250
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic202179e_si_001_06.cif
_cod_data_source_block           1562
_cod_database_code               4328010