The Hexaazidosilicate(IV) Ion: Synthesis, Properties, and Molecular Structure
Alexander C. Filippou; Peter Portius; Gregor Schnakenburg; Journal of the American Chemical Society 124 (2002) 12396–12397; doi:10.1021/ja0273187

data_4115215
_publ_section_title
;
 The Hexaazidosilicate(IV) Ion: Synthesis, Properties, and Molecular
 Structure
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12396
_journal_page_last               12397
_journal_paper_doi               10.1021/ja0273187
_journal_volume                  124
_journal_year                    2002
_chemical_formula_moiety         '2(C36 H30 N P2), N18 Si'
_chemical_formula_sum            'C72 H60 N20 P4 Si'
_chemical_formula_weight         1357.37
_chemical_melting_point          498(2)
_chemical_name_common
;
 Bis(bis(triphenylphosphiniminium))hexaazidosilicate
;
_chemical_name_systematic
;
Bis(bis(P,P,P-triphenylphosphinimidato-\kN)phosphor(1+))
hexaazidosilicate(2-)
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_contact_author_address
;
    Alexander C. Filippou
    Humboldt-Universit\"at zu Berlin   
    Institut f\"ur Anorganische und Allgemeine Chemie
    Brook-Taylor-Str. 2
    D-12489 Berlin
    Germany
;
_audit_contact_author_email      filippou@chemie.hu-berlin.de
_audit_contact_author_fax        '(+49) 030 2093-6939'
_audit_contact_author_phone      '(+49) 030 2093-7385'
_audit_creation_date             02-06-07
_audit_creation_method           SHELXL-97
_cell_angle_alpha                64.55(2)
_cell_angle_beta                 71.10(2)
_cell_angle_gamma                75.691(18)
_cell_formula_units_Z            1
_cell_length_a                   11.560(2)
_cell_length_b                   12.839(3)
_cell_length_c                   13.468(4)
_cell_measurement_reflns_used    30
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      12.4
_cell_measurement_theta_min      11.5
_cell_volume                     1693.9(8)
_computing_cell_refinement       'STADI4 (STOE, 1996)'
_computing_data_collection       'STADI4 (STOE, 1996)'
_computing_data_reduction        'X-RED 1.08a (STOE, 1996)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 1996)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997) CIFTAB'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      180(2)
_diffrn_detector_area_resol_mean none
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'STOE Stadi4 Diffractometer'
_diffrn_measurement_method
; 
Scan width (omega) = 1.25 - 1.40, scan ratio 2theta:omega = 1.00
I(Net) and sigma(I) calculated according to Blessing (1987)
;
_diffrn_radiation_collimation    '0.8 mm'
_diffrn_radiation_detector       'NaI(Tl) Scintillation Counter'
_diffrn_radiation_monochromator  'Planar Graphite'
_diffrn_radiation_polarisn_norm  90
_diffrn_radiation_source         'fine-focus sealed X-ray tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  none
_diffrn_reflns_av_sigmaI/netI    0.0179
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            7721
_diffrn_reflns_theta_full        27.44
_diffrn_reflns_theta_max         27.44
_diffrn_reflns_theta_min         1.73
_diffrn_standards_decay_%        1.8
_diffrn_standards_interval_count 26
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.189
_exptl_absorpt_correction_T_max  0.9030
_exptl_absorpt_correction_T_min  0.8757
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.331
_exptl_crystal_description       prism
_exptl_crystal_F_000             706
_exptl_crystal_size_max          0.72
_exptl_crystal_size_mid          0.60
_exptl_crystal_size_min          0.55
_refine_diff_density_max         0.506
_refine_diff_density_min         -0.308
_refine_diff_density_rms         0.045
_refine_ls_extinction_coef       0.0075(8)
_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   1.044
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     530
_refine_ls_number_reflns         7721
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0419
_refine_ls_R_factor_gt           0.0330
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0428P)^2^+0.7459P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0814
_refine_ls_wR_factor_ref         0.0887
_reflns_number_gt                6638
_reflns_number_total             7721
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0273187-2_s2.cif
_cod_data_source_block           port18
_cod_original_cell_volume        1693.9(7)
_cod_database_code               4115215