Spectroscopic and Structural Studies of Difluorophosphoryl Azide F2P(O)N3, Difluorophosphoryl Isocyanate F2P(O)NCO, and Difluorophosphoric Acid Anhydride, F2(O)POP(O)F2
Xiaoqing Zeng; Michael Gerken; Helmut Beckers; Helge Willner; Inorganic Chemistry 49 (2010) 3002–3010; doi:10.1021/ic902524u

data_4315201
_publ_contact_author_address
;FB C-Anorganische Chemie
Bergische Universitaet Wuppertal
Gaussstr. 20
42097 Wuppertal
Germany
;
_publ_contact_author_email       willner@uni-wuppertal.de
_publ_contact_author_name        'Helge Willner'
_publ_section_title
;
 Spectroscopic and Structural Studies of Difluorophosphoryl Azide
 F2P(O)N3, Difluorophosphoryl Isocyanate F2P(O)NCO, and Difluorophosphoric
 Acid Anhydride, F2(O)POP(O)F2
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3002
_journal_page_last               3010
_journal_paper_doi               10.1021/ic902524u
_journal_volume                  49
_journal_year                    2010
_chemical_formula_sum            'C F2 N O2 P'
_chemical_formula_weight         126.99
_space_group_IT_number           82
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'I -4'
_symmetry_space_group_name_H-M   'I -4'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   12.9771(6)
_cell_length_b                   12.9771(6)
_cell_length_c                   4.9718(3)
_cell_measurement_reflns_used    590
_cell_measurement_temperature    135(2)
_cell_measurement_theta_max      29.4259
_cell_measurement_theta_min      3.1334
_cell_volume                     837.28(7)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.42 (release 29-05-2009 CrysAlis171 .NET)
(compiled May 29 2009,17:40:42)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.42 (release 29-05-2009 CrysAlis171 .NET)
(compiled May 29 2009,17:40:42)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.42 (release 29-05-2009 CrysAlis171 .NET)
(compiled May 29 2009,17:40:42)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      135(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_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0160
_diffrn_reflns_av_sigmaI/netI    0.0406
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -3
_diffrn_reflns_number            963
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         29.49
_diffrn_reflns_theta_min         3.14
_exptl_absorpt_coefficient_mu    0.582
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.90999
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.42 (release 29-05-2009 CrysAlis171 .NET)
(compiled May 29 2009,17:40:42)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.015
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             496
_exptl_crystal_size_max          0.167
_exptl_crystal_size_mid          0.041
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.215
_refine_diff_density_min         -0.233
_refine_diff_density_rms         0.051
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.77(17)
_refine_ls_extinction_coef       0.0056(11)
_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   0.877
_refine_ls_matrix_type           full
_refine_ls_number_parameters     66
_refine_ls_number_reflns         751
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.877
_refine_ls_R_factor_all          0.0333
_refine_ls_R_factor_gt           0.0274
_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^)+(0.0328P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0560
_refine_ls_wR_factor_ref         0.0574
_reflns_number_gt                647
_reflns_number_total             751
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic902524u_si_002_3.cif
_cod_data_source_block           mg_8c
_cod_original_cell_volume        837.27(8)
_cod_database_code               4315201