Pyramidal Inversion Isomers in the Solid-State Structure of the Tricyclic Antimony-Tellurium Imido Complex TeSb2Cl2(NtBu)4
Tristram Chivers; Gabriele Schatte; Inorganic Chemistry 41 (2002) 1002–1006; doi:10.1021/ic0109694

data_4317586
_publ_contact_author_address
; Department of Chemistry
   University of Calgary
   Calgary Alberta T2N 1N4
   Canada
;
_publ_contact_author_email       chivers@ucalgary.ca
_publ_contact_author_fax         '001 403 289 9488'
_publ_contact_author_name        'Dr Tristram Chivers'
_publ_contact_author_phone       '001 403 220 5741'
_publ_section_title
;
 Pyramidal Inversion Isomers in the Solid-State Structure of the Tricyclic
 Antimony-Tellurium Imido Complex TeSb2Cl2(NtBu)4
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1002
_journal_page_last               1006
_journal_paper_doi               10.1021/ic0109694
_journal_volume                  41
_journal_year                    2002
_chemical_formula_moiety         'C12 H28 Cl2 N3 Sb Te, C7H8'
_chemical_formula_sum            'C19 H36 Cl2 N3 Sb Te'
_chemical_formula_weight         626.76
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 99.693(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.9127(17)
_cell_length_b                   11.7159(14)
_cell_length_c                   15.8789(19)
_cell_measurement_reflns_used    3741
_cell_measurement_temperature    193(2)
_cell_volume                     2551.3(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'ORTEP-3 (1.05) in WinGX-1.62'
_computing_publication_material  WinGX-1.62
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0450
_diffrn_reflns_av_sigmaI/netI    0.0429
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            9674
_diffrn_reflns_theta_full        23.26
_diffrn_reflns_theta_max         23.26
_diffrn_reflns_theta_min         1.80
_diffrn_standards_decay_%        'no decay'
_exptl_absorpt_coefficient_mu    2.420
_exptl_absorpt_correction_T_max  0.7600
_exptl_absorpt_correction_T_min  0.3959
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;SADABS, V 2.01, Software for Area-Detector Absorption
   Corrections; Bruker AXS Inc., Madison, WI, 2000.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.632
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1232
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.12
_refine_diff_density_max         2.476
_refine_diff_density_min         -0.810
_refine_diff_density_rms         0.142
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     249
_refine_ls_number_reflns         3630
_refine_ls_number_restraints     52
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.0745
_refine_ls_R_factor_gt           0.0556
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0629P)^2^+21.2421P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1449
_refine_ls_wR_factor_ref         0.1579
_reflns_number_gt                2783
_reflns_number_total             3630
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0109694_1.cif
_cod_data_source_block           4
_cod_database_code               4317586