Synthesis and Characterization of the First Azastibatranes and Azabismatranes
Pavel L. Shutov; Sergey S. Karlov; Klaus Harms; Daniil A. Tyurin; Andrei V. Churakov; Jörg Lorberth; Galina S. Zaitseva; Inorganic Chemistry 41 (2002) 6147–6152; doi:10.1021/ic0257423

data_4318861
_publ_section_title
;
 Synthesis and Characterization of the First Azastibatranes and
 Azabismatranes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6147
_journal_page_last               6152
_journal_paper_doi               10.1021/ic0257423
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C15 H39 N4 Sb Si3'
_chemical_formula_weight         481.52
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           148
_symmetry_cell_setting           rhombohedral
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_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                120.00
_cell_formula_units_Z            6
_cell_length_a                   16.2434(7)
_cell_length_b                   16.2434(7)
_cell_length_c                   15.482(1)
_cell_measurement_temperature    193(2)
_cell_volume                     3537.6(3)
_computing_cell_refinement       'Stoe Cell'
_computing_data_collection       'Stoe Expose'
_computing_data_reduction        'Stoe Integrate'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens 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  'Stoe IPDS'
_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  0.0277
_diffrn_reflns_av_sigmaI/netI    0.0102
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            17246
_diffrn_reflns_theta_full        27.44
_diffrn_reflns_theta_max         27.44
_diffrn_reflns_theta_min         1.96
_exptl_absorpt_coefficient_mu    1.327
_exptl_absorpt_correction_T_max  0.7680
_exptl_absorpt_correction_T_min  0.6056
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.356
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1500
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.573
_refine_diff_density_min         -0.518
_refine_diff_density_rms         0.092
_refine_ls_extinction_coef       0.00117(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.287
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     123
_refine_ls_number_reflns         1790
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.287
_refine_ls_R_factor_all          0.0206
_refine_ls_R_factor_gt           0.0176
_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^)+(0.0131P)^2^+12.6574P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0451
_refine_ls_wR_factor_ref         0.0598
_reflns_number_gt                1673
_reflns_number_total             1790
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0257423-2_s3.cif
_cod_data_source_block           shut06
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Rhombohedral' changed to
'rhombohedral' according to the built-in table from CIF Core
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        3537.7(3)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               4318861