Synthesis and Characterization of the Phosphorus Triazides OP(N3)3 and SP(N3)3
Xiaoqing Zeng; Eduard Bernhardt; Helmut Beckers; Helge Willner; Inorganic Chemistry 50 (2011) 11235–11241; doi:10.1021/ic201802x

data_4326765
_publ_contact_author_address
;
 Bergische Universit\"at Wuppertal
 FB C - Anorganische Chemie
 Gau\&sstr. 20
 D-42097 Wuppertal
;
_publ_contact_author_email       zeng@uni-wuppertal.de
_publ_contact_author_name        'Xiaoqing Zeng'
_publ_section_title
;
 Synthesis and Characterization of the Phosphorus Triazides OP(N3)3 and
 SP(N3)3
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11235
_journal_page_last               11241
_journal_paper_doi               10.1021/ic201802x
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         'N9 O P'
_chemical_formula_sum            'N9 O P'
_chemical_formula_weight         173.06
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2011-07-01 # Formatted by publCIF
;
_cell_angle_alpha                90.00
_cell_angle_beta                 111.918(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.0591(4)
_cell_length_b                   12.1904(5)
_cell_length_c                   7.7482(4)
_cell_measurement_reflns_used    992
_cell_measurement_temperature    140(2)
_cell_measurement_theta_max      28.9237
_cell_measurement_theta_min      3.3304
_cell_volume                     618.56(6)
_computing_cell_refinement       'CrysAlisPro171.34.49, Oxford Diffraction'
_computing_data_collection       'CrysAlisPro171.34.49, Oxford Diffraction'
_computing_data_reduction        'CrysAlisPro171.34.49, Oxford Diffraction'
_computing_molecular_graphics    'Diamond, v.2.1e (Brandenburg, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      140(2)
_diffrn_detector_area_resol_mean 16.2705
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.847
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w 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  0.0145
_diffrn_reflns_av_sigmaI/netI    0.0224
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            2599
_diffrn_reflns_theta_full        26.40
_diffrn_reflns_theta_max         29.18
_diffrn_reflns_theta_min         3.11
_exptl_absorpt_coefficient_mu    0.400
_exptl_absorpt_correction_T_max  0.950
_exptl_absorpt_correction_T_min  0.829
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.858
_exptl_crystal_description       prism
_exptl_crystal_F_000             344
_exptl_crystal_size_max          0.74
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.287
_refine_diff_density_min         -0.333
_refine_diff_density_rms         0.056
_refine_ls_extinction_coef       0.043(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_matrix_type           full
_refine_ls_number_parameters     101
_refine_ls_number_reflns         1420
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0282
_refine_ls_R_factor_gt           0.0254
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0377P)^2^+0.1360P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0684
_refine_ls_wR_factor_ref         0.0708
_reflns_number_gt                1283
_reflns_number_total             1420
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic201802x_si_002_2.cif
_cod_data_source_block           exp_1798
_cod_original_sg_symbol_Hall     '-P 2ybc '
_cod_database_code               4326765