TAS+(Z)-Me3CNSN- and TAS+(E)-Me3SiNSN-: Does the Anion-Cation Interaction Influence the Configuration?
Tobias Borrmann; Andrey V. Zibarev; Enno Lork; Gerd Knitter; Shan-Jia Chen; Paul G. Watson; Edgardo Cutin; Makhmut M. Shakirov; Wolf-Dieter Stohrer; Rüdiger Mews; Inorganic Chemistry 39 (2000) 3999–4005; doi:10.1021/ic0004030

data_4321337
_publ_section_title
;
 TAS+(Z)-Me3CNSN- and TAS+(E)-Me3SiNSN-: Does the Anion-Cation Interaction
 Influence the Configuration?
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3999
_journal_page_last               4005
_journal_paper_doi               10.1021/ic0004030
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C9 H27 N5 S2 Si'
_chemical_formula_weight         297.57
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_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                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.216(2)
_cell_length_b                   11.0890(10)
_cell_length_c                   7.2870(10)
_cell_measurement_reflns_used    33
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      14.992
_cell_measurement_theta_min      8.656
_cell_volume                     1714.4(3)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens XSCANS'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Siemens P4'
_diffrn_measurement_method       '2\q/\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0348
_diffrn_reflns_av_sigmaI/netI    0.0484
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       1
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            2803
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.66
_diffrn_standards_decay_%        'random variation +/-2.0'
_diffrn_standards_interval_count 197
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.372
_exptl_absorpt_correction_T_max  0.8360
_exptl_absorpt_correction_T_min  0.7810
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.153
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             648
_exptl_crystal_size_max          0.70
_exptl_crystal_size_mid          0.60
_exptl_crystal_size_min          0.50
_refine_diff_density_max         0.211
_refine_diff_density_min         -0.351
_refine_diff_density_rms         0.050
_refine_ls_extinction_coef       0.0084(13)
_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   0.978
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     101
_refine_ls_number_reflns         2069
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.978
_refine_ls_R_factor_all          0.0477
_refine_ls_R_factor_gt           0.0347
_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^)+(0.0526P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0920
_refine_ls_wR_factor_ref         0.0957
_reflns_number_gt                1551
_reflns_number_total             2069
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0004030.cif
_cod_data_source_block           as4
_cod_database_code               4321337