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

data_1513673
_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         'C24 H40 N4 P4, 2(C H2 Cl2)'
_chemical_formula_sum            'C26 H44 Cl4 N4 P4'
_chemical_formula_weight         678.33
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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                111.4080(10)
_cell_angle_beta                 105.6400(10)
_cell_angle_gamma                97.4310(10)
_cell_formula_units_Z            2
_cell_length_a                   11.5705(5)
_cell_length_b                   12.2221(3)
_cell_length_c                   13.6923(3)
_cell_measurement_reflns_used    9574
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      58.578
_cell_measurement_theta_min      5.544
_cell_volume                     1679.03(9)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0507
_diffrn_reflns_av_sigmaI/netI    0.0422
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            46693
_diffrn_reflns_theta_full        29.00
_diffrn_reflns_theta_max         29.00
_diffrn_reflns_theta_min         1.85
_exptl_absorpt_coefficient_mu    0.567
_exptl_absorpt_correction_T_max  0.9455
_exptl_absorpt_correction_T_min  0.8951
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.342
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             712
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.400
_refine_diff_density_min         -0.343
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     380
_refine_ls_number_reflns         8903
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0687
_refine_ls_R_factor_gt           0.0427
_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^)+(0.0563P)^2^+0.6250P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1035
_refine_ls_wR_factor_ref         0.1184
_reflns_number_gt                6414
_reflns_number_total             8903
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c3sc52322e.txt
_cod_data_source_block           ch121_[PN(C6H10)]4
_cod_original_cell_volume        1679.02(9)
_cod_database_code               1513673