First structural characterization of a mixed valent thallium(i/iii) amide bearing an n-butylthallium(iii) unit stabilized by a tripodal amido ligand
Galka, Christian H.; Gade, Lutz H.; Chemical Communications  (2001) 899–; doi:10.1039/b100760m

data_7114848
_publ_contact_author
; 
Prof. Dr. Lutz H. Gade 
Laboratoire de Chimie Organometallique et de Catalyse (UMR 7513) 
Institut LeBel 
Universite Louis Pasteur 
4, rue Blaise Pascal 
67070 Strasbourg 
France 
;
_publ_section_title
;
 First structural characterization of a mixed valent thallium(i/iii) amide
 bearing an n-butylthallium(iii) unit stabilized by a tripodal amido
 ligand
;
_journal_issue                   10
_journal_name_full               'Chemical Communications'
_journal_page_first              899
_journal_paper_doi               10.1039/b100760m
_journal_year                    2001
_chemical_formula_sum            'C34.5 H55 N3 Si3 Tl2'
_chemical_formula_weight         1004.83
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 107.869(14)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   21.346(6)
_cell_length_b                   14.4015(13)
_cell_length_c                   26.384(10)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      10
_cell_volume                     7720(4)
_computing_cell_refinement       'CAD4 (Enraf-Nonius)'
_computing_data_collection       'CAD4 (Enraf-Nonius)'
_computing_data_reduction        'BEGIN (SDP)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CAD4 (Enraf-Nonius)'
_diffrn_measurement_method       'Omega/Theta scans'
_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  0.0423
_diffrn_reflns_av_sigmaI/netI    0.0412
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       1
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       2
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            7684
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         2.00
_diffrn_standards_decay_%        1.6
_diffrn_standards_interval_time  60
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    8.459
_exptl_absorpt_correction_T_max  0.9991
_exptl_absorpt_correction_T_min  0.3611
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
; 
empirical absorption correction by psi-scans from 10 reflections 
with chi-angles near 90 degrees 
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.729
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3896
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         2.214
_refine_diff_density_min         -2.920
_refine_diff_density_rms         0.220
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     382
_refine_ls_number_reflns         6781
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0693
_refine_ls_R_factor_gt           0.0471
_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^)+(0.0653P)^2^+88.4538P] where P==(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1108
_refine_ls_wR_factor_ref         0.1287
_reflns_number_gt                5138
_reflns_number_total             6781
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b100760m.txt
_cod_data_source_block           2
_cod_original_cell_volume        7719(4)
_cod_original_formula_sum        'C34.50 H55 N3 Si3 Tl2'
_cod_database_code               7114848