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_2101952
_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         'C Cl7 N2 P2 1+, Cl6 P 1-'
_chemical_formula_structural     '(Cl C(N P Cl3)2) (P Cl6)'
_chemical_formula_sum            'C Cl13 N2 P3'
_chemical_formula_weight         593.83
_chemical_melting_point          441.15
_chemical_name_common
;
 Chloro-bis(trichlorophosphazeno)methyl hexachlorophosphate
;
_chemical_name_systematic
;
 [N-(chloroformimidoyl)phosphorimidic trichloridato]trichlorophosphorus
 hexachlorophosphate
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 96.900(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.958(2)
_cell_length_b                   11.546(2)
_cell_length_c                   15.726(2)
_cell_measurement_reflns_used    53
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      19.5
_cell_measurement_theta_min      15.0
_cell_volume                     1795.0(5)
_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  0.0274
_diffrn_reflns_av_sigmaI/netI    0.0391
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            12747
_diffrn_reflns_theta_max         40.00
_diffrn_reflns_theta_min         1.30
_diffrn_standards_decay_%        1.02
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.250
_exptl_absorpt_correction_T_max  0.844
_exptl_absorpt_correction_T_min  0.630
_exptl_absorpt_correction_type   refdelf
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    2.197
_exptl_crystal_description       block
_exptl_crystal_F_000             1144
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.629
_refine_diff_density_min         -0.738
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.12(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.063
_refine_ls_goodness_of_fit_obs   1.052
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         12231
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.110
_refine_ls_restrained_S_obs      1.052
_refine_ls_R_factor_all          0.0433
_refine_ls_R_factor_obs          0.0313
_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^)+(0.0398P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0854
_refine_ls_wR_factor_obs         0.0748
_reflns_number_observed          10519
_reflns_number_total             12281
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            se0217.cif
_cod_data_source_block           p26
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '168_C' was changed to '441.15' - 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 '168_C' was changed to '441.15' - 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^)+(0.0398P)^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^)+(0.0398P)^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_original_sg_symbol_Hall     'P 2y1'
_cod_database_code               2101952