Structures of the Phosphazenes [ClC(NPCl~3~)~2~]^+^PCl~6~^{-^} and [CH~3~C(NPCl~3~)~2~]^+^SbCl~6~^{-^} at 90 K
Belaj, F.; Acta Crystallographica Section B 53 (1997) 953–960; doi:10.1107/S0108768197008343

data_2101953
_publ_section_title
;
 Structures of the Phosphazenes [ClC(NPCl~3~)~2~]^+^PCl~6~^{-^} and
 [CH~3~C(NPCl~3~)~2~]^+^SbCl~6~^{-^} at 90 K
;
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              953
_journal_page_last               960
_journal_paper_doi               10.1107/S0108768197008343
_journal_volume                  53
_journal_year                    1997
_chemical_formula_moiety         'C2 H3 Cl6 N2 P2 1+, Cl6 Sb 1-'
_chemical_formula_structural     '(C H3 C(N P Cl3)2) (Sb Cl6)'
_chemical_formula_sum            'C2 H3 Cl12 N2 P2 Sb'
_chemical_formula_weight         664.19
_chemical_melting_point          453.15
_chemical_name_common
;
 Methyl-bis(trichlorophosphazeno)methyl hexachloroantimonate
;
_chemical_name_systematic
;
 [N-(acetimidoyl) phosphorimidic trichloridato]trichlorophosphorus
 hexachloroantimonate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.090(10)
_cell_angle_beta                 91.170(10)
_cell_angle_gamma                108.860(10)
_cell_formula_units_Z            4
_cell_length_a                   12.1330(10)
_cell_length_b                   12.2290(10)
_cell_length_c                   13.975(2)
_cell_measurement_reflns_used    70
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      18.4
_cell_measurement_theta_min      15.6
_cell_volume                     1961.7(4)
_computing_cell_refinement       'local program'
_computing_data_collection       'local program'
_computing_data_reduction        'local program'
_computing_molecular_graphics    'ORTEP (Johnson, 1965)'
_computing_publication_material  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1985)'
_diffrn_ambient_temperature      90(2)
_diffrn_measurement_device       'Stoe 4-circle diffractometer'
_diffrn_measurement_method       'profile data from omega - scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0263
_diffrn_reflns_av_sigmaI/netI    0.0466
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            12700
_diffrn_reflns_theta_max         30.02
_diffrn_reflns_theta_min         2.88
_diffrn_standards_decay_%        1.48
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.189
_exptl_absorpt_correction_T_max  0.876
_exptl_absorpt_correction_T_min  0.563
_exptl_absorpt_correction_type   refdelf
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    2.249
_exptl_crystal_description       block
_exptl_crystal_F_000             1256
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.045
_refine_diff_density_min         -1.270
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.033
_refine_ls_goodness_of_fit_obs   1.075
_refine_ls_hydrogen_treatment
'common Uiso for each rigid CH3 group (AFIX 35)'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     365
_refine_ls_number_reflns         11416
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_restrained_S_obs      1.075
_refine_ls_R_factor_all          0.0481
_refine_ls_R_factor_obs          0.0357
_refine_ls_shift/esd_max         -0.002
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0422P)^2^+2.0943P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0932
_refine_ls_wR_factor_obs         0.0861
_reflns_number_observed          9316
_reflns_number_total             11420
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            se0217.cif
_cod_data_source_block           ch3p26
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '180_C' was changed to '453.15' - it
was converted from degrees Celsius(C) to Kelvins(K).

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_chemical_melting_point' value '180_C' was changed to '453.15' - it
was converted from degrees Celsius(C) to Kelvins(K).

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0422P)^2^+2.0943P] 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^)+(0.0422P)^2^+2.0943P] 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               2101953