1,3-Diphenyl-2,2,2,4,4,4-hexazido-1,3-diaza-2,4-diphosphetidine: synthesis and structural characterisation of the first nitrogen-penta-coordinated phosphorus with three azide-groups
Aubauer, Christoph; Klapötke, Thomas M.; Nöth, Heinrich; Schulz, Axel; Suter, Max; Weigand, Jan; Chemical Communications  (2000) 2491–; doi:10.1039/b006944m

data_7111111
_publ_contact_author
;
      Heinrich N\"oth
      Institut f\"ur anorganische Chemie
      Universit\"at M\"unchen
      Butenandtstr. 5-13 (Haus D)
      81377 M\"unchen
      Bundesrepublik Deutschland
;
_publ_section_title
;
 1,3-Diphenyl-2,2,2,4,4,4-hexazido-1,3-diaza-2,4-diphosphetidine:
 synthesis and structural characterisation of the first
 nitrogen-penta-coordinated phosphorus with three azide-groups
;
_journal_issue                   24
_journal_name_full               'Chemical Communications'
_journal_page_first              2491
_journal_paper_doi               10.1039/b006944m
_journal_year                    2000
_chemical_formula_sum            'C12 H10 N20 P2'
_chemical_formula_weight         496.34
_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-CIF-file updated by CIFRTF'
_cell_angle_alpha                88.527(3)
_cell_angle_beta                 85.499(4)
_cell_angle_gamma                67.684(3)
_cell_formula_units_Z            2
_cell_length_a                   7.3415(15)
_cell_length_b                   8.5508(18)
_cell_length_c                   17.879(4)
_cell_measurement_reflns_used    323
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      1.00
_cell_measurement_theta_min      20.00
_cell_volume                     1035.1(4)
_computing_cell_refinement       'SMART (V4.C50)'
_computing_data_collection       'SMART (V4.C50)'
_computing_data_reduction        'SAINT (V4.D50)'
_computing_molecular_graphics    'XP (SHELXTL-Ver.5)'
_computing_publication_material  'SHELXL (Sheldrick 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.597
_diffrn_measured_fraction_theta_max 0.597
_diffrn_measurement_device_type  'Siemens SMART Area-detector'
_diffrn_measurement_method       Hemisphere
_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  0.0408
_diffrn_reflns_av_sigmaI/netI    0.0818
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            5983
_diffrn_reflns_theta_full        28.56
_diffrn_reflns_theta_max         28.56
_diffrn_reflns_theta_min         1.14
_diffrn_standards_interval_time  0
_exptl_absorpt_coefficient_mu    0.262
_exptl_absorpt_correction_T_max  0.9828
_exptl_absorpt_correction_T_min  0.6491
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.592
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             504
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.311
_refine_diff_density_min         -0.337
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.879
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     307
_refine_ls_number_reflns         3153
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.879
_refine_ls_R_factor_all          0.0920
_refine_ls_R_factor_gt           0.0488
_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^)+(0.0724P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1148
_refine_ls_wR_factor_ref         0.1273
_reflns_number_gt                1830
_reflns_number_total             3153
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b006944msup1.cif
_cod_data_source_block           auba4
_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 2.4.2 from
2011-04-26.

'_refine_ls_hydrogen_treatment' value 'mixed ' changed
to 'mixed' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'direct methods' was changed to
'direct'.

'_atom_sites_solution_hydrogens' value 'geometrically' was changed to
'geom'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7111111