Diatomic PN – trapped in a cyclo-tetraphosphazene
Hering, Christian; Schulz, Axel; Villinger, Alexander; Chemical Science 5 (2014) 1064–; doi:10.1039/c3sc52322e

data_1513678
_publ_section_title
;
 Diatomic PN -- trapped in a cyclo-tetraphosphazene
;
_journal_issue                   3
_journal_name_full               'Chemical Science'
_journal_page_first              1064
_journal_paper_doi               10.1039/c3sc52322e
_journal_volume                  5
_journal_year                    2014
_chemical_formula_moiety
;
C12 H23 N O P +, C F3 O3 S -, C H2 Cl2
;
_chemical_formula_sum            'C14 H25 Cl2 F3 N O4 P S'
_chemical_formula_weight         462.28
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      33
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_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            4
_cell_length_a                   17.3330(14)
_cell_length_b                   8.3372(6)
_cell_length_c                   14.4037(10)
_cell_measurement_reflns_used    1974
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      41.585
_cell_measurement_theta_min      4.700
_cell_volume                     2081.5(3)
_computing_cell_refinement       'Bruker Apex V7.51A'
_computing_data_collection       'Bruker Apex V7.51A'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'ORTEP-3v2.01 (Farrugia, 1997)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker Apex Kappa II-CCD-diffractometer'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0621
_diffrn_reflns_av_sigmaI/netI    0.0794
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            14093
_diffrn_reflns_theta_full        29.00
_diffrn_reflns_theta_max         29.00
_diffrn_reflns_theta_min         2.35
_exptl_absorpt_coefficient_mu    0.534
_exptl_absorpt_correction_T_max  0.9687
_exptl_absorpt_correction_T_min  0.8310
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.475
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             960
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.485
_refine_diff_density_min         -0.284
_refine_diff_density_rms         0.064
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.29(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.970
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     299
_refine_ls_number_reflns         4994
_refine_ls_number_restraints     38
_refine_ls_restrained_S_all      0.967
_refine_ls_R_factor_all          0.0945
_refine_ls_R_factor_gt           0.0530
_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^)+(0.0597P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1155
_refine_ls_wR_factor_ref         0.1300
_reflns_number_gt                3252
_reflns_number_total             4994
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c3sc52322e.txt
_cod_data_source_block           ch115_2_[P(O)H(C6H10)2NH2]
_cod_database_code               1513678