Synthesis of Volatile Cyclic Silylamines and the Molecular Structures of Two 1-Aza-2,5-disilacyclopentane Derivatives
Norbert W. Mitzel; Hubert Schmidbaur; David W. H. Rankin; Bruce A. Smart; Matthias Hofmann; Paul von Ragué Schleyer; Inorganic Chemistry 36 (1997) 4360–4368; doi:10.1021/ic9703179

data_4323595
_publ_section_title
;
 Synthesis of Volatile Cyclic Silylamines and the Molecular Structures of
 Two 1-Aza-2,5-disilacyclopentane Derivatives
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4360
_journal_page_last               4368
_journal_paper_doi               10.1021/ic9703179
_journal_volume                  36
_journal_year                    1997
_chemical_formula_sum            'C4 H14 N2 Si2'
_chemical_formula_weight         146.35
_chemical_melting_point          160
_chemical_name_systematic
; 
 N-(Dimethylamino)-2,5-disilapyrrolidine 
;
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 95.20(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.050(3)
_cell_length_b                   8.547(4)
_cell_length_c                   9.878(3)
_cell_measurement_reflns_used    44
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      16
_cell_measurement_theta_min      14
_cell_volume                     845.0(5)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      113(2)
_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    0.0411
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            2693
_diffrn_reflns_theta_max         30.04
_diffrn_reflns_theta_min         3.13
_diffrn_standards_decay_%        None
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.338
_exptl_absorpt_correction_T_max  0.846
_exptl_absorpt_correction_T_min  0.711
_exptl_absorpt_correction_type   Psi-scans
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.150
_exptl_crystal_description       Cylinder
_exptl_crystal_F_000             320
_exptl_crystal_size_max          0.8
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.5
_refine_diff_density_max         0.447
_refine_diff_density_min         -0.453
_refine_diff_density_rms         0.071
_refine_ls_extinction_coef       0.1401(75)
_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_all   1.029
_refine_ls_goodness_of_fit_obs   1.075
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     130
_refine_ls_number_reflns         2466
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_restrained_S_obs      1.075
_refine_ls_R_factor_all          0.0605
_refine_ls_R_factor_obs          0.0390
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0564P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0987
_refine_ls_wR_factor_obs         0.0890
_reflns_number_observed          1888
_reflns_number_total             2467
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9703179.cif
_cod_data_source_block           si2hyd
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0564P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0564P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4323595