Experimental Investigations and ab Initio Studies on Hexacoordinated Complexes of Dichlorosilane
Karl Hensen; Thorsten Stumpf; Michael Bolte; Christian Näther; Holger Fleischer; Journal of the American Chemical Society 120 (1998) 10402–10408; doi:10.1021/ja981016g

data_4116846
_publ_contact_author
;
      Dr. Michael Bolte
      Institut f\"ur Organische Chemie
      J.-W.-Goethe-Universit\"at
      Marie-Curie-Str. 11
      60439 Frankfurt/Main
      Germany
;
_publ_contact_author_email       bolte@chemie.uni-frankfurt.de
_publ_contact_author_fax         '49 69 798 29128'
_publ_contact_author_phone       '49 69 798 29136'
_publ_section_title
;
 Experimental Investigations and ab Initio Studies on Hexacoordinated
 Complexes of Dichlorosilane
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10402
_journal_page_last               10408
_journal_paper_doi               10.1021/ja981016g
_journal_volume                  120
_journal_year                    1998
_chemical_formula_sum            'C10 H12 Cl2 N2 Si'
_chemical_formula_weight         259.21
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_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
_cell_angle_alpha                90
_cell_angle_beta                 118.576(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.4608(1)
_cell_length_b                   6.1660(1)
_cell_length_c                   14.3313(2)
_cell_measurement_reflns_used    4567
_cell_measurement_temperature    153
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      1.00
_cell_volume                     1199.79(3)
_computing_cell_refinement       'Siemens SMART'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens SAINT'
_computing_molecular_graphics    'XP (Siemens XTL-Plus)'
_computing_structure_refinement  'SHELXL-96 (Sheldrick, 1996)'
_computing_structure_solution    'SHELXS-96 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153
_diffrn_measurement_device       'Siemens CCD three circle diffractometer'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  'highly oriented graphite crystal'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0361
_diffrn_reflns_av_sigmaI/netI    0.0259
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            7430
_diffrn_reflns_theta_max         26.33
_diffrn_reflns_theta_min         3.00
_diffrn_standards_decay_%        0.0
_diffrn_standards_interval_time  600
_diffrn_standards_number         123
_exptl_absorpt_coefficient_mu    0.609
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7140
_exptl_absorpt_correction_type   'empirical using SADABS (G. Sheldrick)'
_exptl_crystal_colour            'colourless transparent'
_exptl_crystal_density_diffrn    1.435
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    N/A
_exptl_crystal_description       plate
_exptl_crystal_F_000             536
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.213
_refine_diff_density_min         -0.326
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.116
_refine_ls_goodness_of_fit_obs   1.145
_refine_ls_hydrogen_treatment    'see experimental section'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     74
_refine_ls_number_reflns         1203
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.116
_refine_ls_restrained_S_obs      1.145
_refine_ls_R_factor_all          0.0401
_refine_ls_R_factor_obs          0.0289
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0310P)^2^+0.9756P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0696
_refine_ls_wR_factor_obs         0.0656
_reflns_number_observed          1025
_reflns_number_total             1203
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja981016g_2.cif
_cod_data_source_block           he10
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'N/A' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0310P)^2^+0.9756P] 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^)+(0.0310P)^2^+0.9756P] 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               4116846