Experimental and Theoretical Characterization of the Hexaazidophosphate(V) Ion
P. Portius; P. W. Fowler; H. Adams; T. Z. Todorova; Inorganic Chemistry 47 (2008) 12004–12009; doi:10.1021/ic801536z

data_4306723
_publ_contact_author_address
;
Department of Chemistry, University of Sheffield
Brook Hill, Sheffield S3 7HF, UK
;
_publ_contact_author_email       peter.portius@sheffield.ac.uk
_publ_contact_author_fax         '+44 (0)114-22-29346'
_publ_contact_author_name        'Peter Portius'
_publ_contact_author_phone       '+44 (0)114-22-29385'
_publ_section_title
;
Experimental and Theoretical Characterization of the Hexaazidophosphate(V)
Ion
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              12004
_journal_page_last               12009
_journal_paper_doi               10.1021/ic801536z
_journal_volume                  47
_journal_year                    2008
_chemical_formula_moiety         'C36 H30 N P2, N18 P'
_chemical_formula_sum            'C36 H30 N19 P3'
_chemical_formula_weight         821.70
_chemical_melting_point          474
_chemical_name_common            PPN-Hexaazidophosphate
_chemical_name_systematic
;
bis(triphenylphosphoranylidene)ammonium hexakis(azido)phosphate 
;
_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_creation_method           SHELXL-97
_cell_angle_alpha                92.635(5)
_cell_angle_beta                 93.437(5)
_cell_angle_gamma                92.105(4)
_cell_formula_units_Z            1
_cell_length_a                   9.6269(9)
_cell_length_b                   9.8158(9)
_cell_length_c                   10.1414(10)
_cell_measurement_reflns_used    7906
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      19.16
_cell_measurement_theta_min      2.21
_cell_volume                     954.83(16)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 100
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0277
_diffrn_reflns_av_sigmaI/netI    0.0262
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            16811
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.31
_diffrn_reflns_theta_min         2.08
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.213
_exptl_absorpt_correction_T_max  0.9708
_exptl_absorpt_correction_T_min  0.9349
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.429
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       PRISM
_exptl_crystal_F_000             424
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.610
_refine_diff_density_min         -0.316
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     265
_refine_ls_number_reflns         4674
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0452
_refine_ls_R_factor_gt           0.0385
_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^)+(0.0675P)^2^+0.2521P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1031
_refine_ls_wR_factor_ref         0.1082
_reflns_number_gt                4070
_reflns_number_total             4674
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic801536z_si_002.cif
_cod_data_source_block           ch1ppx1_0m
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
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_cod_original_sg_symbol_Hall     -P1
_cod_database_code               4306723