Structure and Motion of Tetrakis(trichlorophosphazeno)phosphonium Hexachlorophosphate, [P(NPCl~3~)~4~]^+^PCl~6~^{-^}, at 93 K
Belaj, F.; Acta Crystallographica Section B 53 (1997) 923–927; doi:10.1107/S0108768197005429

data_2101951
_publ_section_title
;
 Structure and Motion of Tetrakis(trichlorophosphazeno)phosphonium
 Hexachlorophosphate, [P(NPCl~3~)~4~]^+^PCl~6~^{-^}, at 93 K
;
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              923
_journal_page_last               927
_journal_paper_doi               10.1107/S0108768197005429
_journal_volume                  53
_journal_year                    1997
_chemical_formula_moiety         'Cl12 N4 P5 1+, Cl6 P 1-'
_chemical_formula_structural     '(P (N P Cl3)4) (P Cl6)'
_chemical_formula_sum            'Cl18 N4 P6'
_chemical_formula_weight         880.02
_chemical_melting_point          542
_chemical_name_systematic
;
 Tetrakis(trichlorophosphazeno)phosphonium hexachlorophosphate
;
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 91.12(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.720(2)
_cell_length_b                   21.235(5)
_cell_length_c                   8.248(2)
_cell_measurement_reflns_used    71
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      15.0
_cell_measurement_theta_min      12.5
_cell_volume                     1351.9(6)
_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, 1990)'
_diffrn_ambient_temperature      93(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  0.0329
_diffrn_reflns_av_sigmaI/netI    0.0658
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            7690
_diffrn_reflns_theta_max         36.00
_diffrn_reflns_theta_min         2.64
_diffrn_standards_decay_%        1.5
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.181
_exptl_absorpt_correction_T_max  1.226
_exptl_absorpt_correction_T_min  0.820
_exptl_absorpt_correction_type   refdelf
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    2.162
_exptl_crystal_description       block
_exptl_crystal_F_000             848
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.307
_refine_diff_density_min         -0.793
_refine_ls_extinction_coef       0.0019(6)
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.007
_refine_ls_goodness_of_fit_obs   1.058
_refine_ls_matrix_type           full
_refine_ls_number_parameters     140
_refine_ls_number_reflns         6415
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_restrained_S_obs      1.058
_refine_ls_R_factor_all          0.0797
_refine_ls_R_factor_obs          0.0497
_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^)+(0.0530P)^2^+0.5323P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1274
_refine_ls_wR_factor_obs         0.1091
_reflns_number_observed          4536
_reflns_number_total             6427
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            se0209.cif
_cod_data_source_block           p50f
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0530P)^2^+0.5323P] 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^)+(0.0530P)^2^+0.5323P] 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_original_sg_symbol_H-M      'P 21/m'
_cod_database_code               2101951